CN105489775B - A kind of photovoltaic material of lamelliform perovskite structure and preparation method thereof - Google Patents
A kind of photovoltaic material of lamelliform perovskite structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of photovoltaic materials of lamelliform perovskite structure and preparation method thereof, belong to photovoltaic material field, particularly belong to the field of the photovoltaic material of perovskite structure.The present invention is by the building-up process of the crystal of perovskite structure, adding in derivant, at appropriate temperature and pH value, is distorted the crystal for being originally used for the perovskite structure of cubic system so as to obtain the crystal that lamelliform stacks the perovskite structure of form.Preparation method process proposed by the present invention is simple, operation is simple, and the crystal electrons efficiency of transmission of obtained lamelliform perovskite structure is high, and photoelectricity high conversion rate during applied in solar cell, loss of electrons is small, and efficiency of transmission is high.
Description
Technical field
The invention belongs to photovoltaic material fields, particularly belong to the field of the photovoltaic material of perovskite structure.
Background technology
Photovoltaic material is the material for referring to convert the solar into electric energy, can predominantly pass through " photovoltaic effect "
The semi-conducting material of electric energy is converted the solar into, including monocrystalline silicon, polysilicon, non-crystalline silicon, GaAs, InP, CdS, CdTe etc..
The optoelectronic transformation efficiency of wherein silica-base material is relatively high, but its manufacture cost is also higher simultaneously, and the semi-conducting materials such as GaAs
Raw material is rare, preparation efficiency is low, stability is poor, has been more limited in practical applications.
The material of perovskite structure in 2009 for the first time as photovoltaic material application, raw material be generally cheap lead,
Halogen and amine salt, the energy gap of material is smaller, shows good application prospect, and optoelectronic transformation efficiency is from initial 3.8%
It develops to 15.9% and has only used time less than 5 years, gradually close to the efficiency of silicon-based photovoltaic material, some scholars are further
Foretell that its electricity conversion more than the photovoltaic material of monocrystalline silicon class, will reach 30% quickly.
When the material for using perovskite structure is as photovoltaic material, at present using it is more be by complete perovskite knot
Method that the solution of the crystal of structure is coated in substrate or by the crystal load of complete perovskite structure in can improve
Dispersibility, increase opto-electronic conversion area are capable of providing on the carrier of electron propagation ducts simultaneously, as publication No. is
The Chinese patent document of CN104091888A《A kind of perovskite structure type solar cell and preparation method thereof》In propose one
Perovskite crystal is carried on TiO by kind2Technical solution in mesoporous, this technical solution increase perovskite crystal in the application
Effective conversion area, increase electron propagation ducts, partly solve the defects of crystalloid solution directly coats, can obtain higher
Theoretical efficiency, but the program still needs the preparation by means of new material, and process is more complicated, and interference may be larger.
The crystal of perovskite structure is mostly cubic system or octahedra crystallographic system, and compound with regular structure is tight, as photovoltaic material
Material can directly generate photogenerated current effective ratio area when using is smaller, under the action of an external electric field in electronic transmission process
Directionality is not ideal enough, it may appear that the loss of part electronics, if can increase it directly generates effective specific surface of photogenerated current
Product, enhances the directionality of electron-transport, the crystal of perovskite structure will be further improved on the basis of existing as photovoltaic
Electricity conversion during materials'use.
The form for adjusting crystal is a kind of relatively effective means for changing crystal property, and common method includes causing brilliant
Lattice distort and crystal transfer, can be induced and generated by chemical/biological derivant, can also be directly by changing reaction temperature
It spends, be heat-treated, applying the modes such as external force effect and generate, wherein changing reaction temperature, carrying out the mode such as being heat-treated and belong to object
Reason acts on, and capacity volume variance is little between being generally chiefly used in different crystal form, in the case of transformation is relatively easy, and uses induction
Agent, which carries out distortion of lattice or crystal transfer, can then produce crystal and be difficult to the form occurred under normal circumstances or be difficult to stable deposit
Form.
The adjustment carried out as needed to crystal habit, derivant can select different types, such as large biological molecule, table
Face activating agent, organic additive etc., after appropriate derivant is determined, the control to reaction process is also extremely important
, because the growth of crystal is a small careful easy process for generating variation, different response parameters will obtain different knots
Fruit can not obtain stable result completely in some cases.
Invention content
Based in the prior art the defects of, the present invention wishes to propose a kind of non-cubic or octahedra crystallographic system, can effectively carry
The photovoltaic material of the perovskite structure of high electricity conversion, and preparation method is disclosed simultaneously, the present invention passes through following technology
Scheme realizes above-mentioned purpose：
The present invention discloses a kind of preparation method of the photovoltaic material of lamelliform perovskite structure first, including following step
Suddenly：
1）The preparation of derivant solution
Cationic surfactant is configured to solution, its a concentration of CMC value of the solution using solvent deionized water
200%~300% to get to derivant solution；
2）The synthesis of presoma
The derivant solution is warming up to 30~40 DEG C, keeps the temperature, it is molten to the derivant under stirring
Halogenation methylamine organic solution is slowly added dropwise in liquid, fast drop lead halide organic solution, the two obtain after mixing again thereafter
The mixed liquor is warming up to 70~90 DEG C, stops stirring, 5~10min stood, thereafter using 2~5 DEG C/min's by mixed liquor
The mixed liquor is cooled to 30~40 DEG C by rate of temperature fall, and it is 10 to add in pH adjusting agent to adjust its pH value into the mixed liquor
Precursor solution is obtained after~14,20~30min of gentle agitation；
3）Crystal cures
The precursor solution is stood into 24~48h at room temperature, is followed by filtered, obtained solid is carried out a large amount of
It is secondary or water rinses three times, it is dried thereafter to get to the photovoltaic material of the lamelliform perovskite structure.
Above-mentioned steps 1）In the critical micelle concentration of surfactant that refers to of CMC value, only on the concentration when,
Surfactant molecule can form micella in the solution, and the concentration of derivant solution is lived compared with cationic surface in the present invention
Property agent CMC value it is high, be because the addition of other solution such as halogenation methylamine organic solution, lead halide organic solution can shadow
The Assembling Behavior of cationic surfactant in the solution is rung, cationic surfactant is equal in whole preparation process if wishing
Stable micellar conformation can be kept, the concentration of cationic surfactant should be one higher in derivant solution herein
Value.
Above-mentioned steps 2）In first in a relatively low temperature（30~40 DEG C）Under sequentially add halogenation methylamine organic solution,
Lead halide organic solution is in order to avoid any one in both solution individually generates stronger physics, change with derivant
Act on and cause finally to cannot get ideal crystal habit, thereafter in a higher temperature（70~90 DEG C）It is lower to stand mixing
Liquid is to make to carry out preliminary synthesis between halogenation methylamine and lead halide, generates basic crystal structure, while this is basic
Crystal structure is not destroyed by external force, and it is in order to which derivant is made to be produced at this stage to crystal growth to cool down again thereafter and adjust pH value
Raw significant impact makes basic crystal structure significantly deviate its original growth pattern that will continue to carry out, non-so as to obtain
Cube or octahedra crystallographic system crystal structure.
Above-mentioned steps 3）In secondary water, the distilled water distilled by second distillation or three times that water refers respectively to three times.
The preferred embodiment of above-mentioned preparation method is：The cationic surfactant is aliphatic ammonium salt.
Its further preferred embodiment is：The cationic surfactant is selected from trimethyl bromination
Ammonium（DTAB）, dodecyl trimethyl ammonium chloride（DTAC）, tetradecyltrimethylammonium bromide（TTAB）, tetradecyltrimethylammonium
Ammonium chloride（TTAC）, cetyl trimethylammonium bromide（CTAB）, hexadecyltrimethylammonium chloride（CTAC）In one kind or
It is a variety of.
Its another preferred embodiment is：The halogenation methylamine is selected from CH3NH3I 、CH3NH3Br、 CH3NH3In Cl
It is one or more.
Its another preferred embodiment is：The halogenation methylamine organic solution is CH3NH3I 、CH3NH3Br、
CH3NH3One or more solution being dissolved in formed in organic solvent in Cl, the organic solvent are gamma-butyrolacton or DMF.
Its another preferred embodiment is：The lead halide is selected from PbCl2、PbBr2、PbI2In it is one or more.
Its another preferred embodiment is：The lead halide organic solution is PbCl2、PbBr2、PbI2In one kind or
A variety of solution being dissolved in formed in organic solvent, the organic solvent are gamma-butyrolacton or n,N-Dimethylformamide
（DMF）.
Its another preferred embodiment is：The pH adjusting agent is in sodium hydroxide, potassium hydroxide, sodium bicarbonate
It is one or more.
Its another preferred embodiment is：A concentration of the 1.0 of lead halide in the halogenation methylamine organic solution~
1.5mol/L；A concentration of 1.0~1.5mol/L of lead halide in the lead halide organic solution.
Present invention further proposes a kind of calcium titaniums being prepared using above-mentioned preparation method and its preferred embodiment
The photovoltaic material of ore deposit structure, crystal are lamelliform.
The photovoltaic material of the perovskite structure is that structural formula is ABX3The crystal by distortion of lattice, wherein A represent
CH3NH3, B represent Pb, X represent Cl, Br, I in it is one or more, crystal structure is in ABX3In the cubic morphology of script in
It is slid on vertical direction, is accordingly changed into lamelliform.
It, can be according to conventional calcium titanium when the photovoltaic material of the lamelliform perovskite structure of the present invention is in solar cell
The use form of the photovoltaic material of ore deposit structure is used as light-absorption layer, and the light of solar cell sun is formed by further assembling
Pole such as assembles to obtain light anode, then with assembling i.e. electrode layer jointly in the way of FTO glass, compacted zone, perovskite successively
Basic solar cell is obtained, the photovoltaic material electron-transport efficiency of lamelliform perovskite structure of the invention is higher, generally
In the case of may not necessarily add in light-absorption layer and additionally between electrode layer hole transmission layer.
The invention has the advantages that：
1）A kind of photovoltaic material of lamelliform perovskite structure has been prepared in the present invention, compared to being originally used for cube or eight
The photovoltaic material of the perovskite structure of face body crystallographic system effectively increases the specific surface area for the material for directly generating photogenerated current,
Under same amount, the electricity conversion higher of the photovoltaic material of lamelliform perovskite structure of the invention being prepared；
2）The photovoltaic material of lamelliform perovskite structure that the present invention is prepared under the action of an external electric field, electron-transport master
It to be carried out on thin layer extending direction, directionality is good, so that its efficiency of transmission is higher；
3）The preparation method process of the present invention is simple, and stability is good, conducive to production.
【Specific embodiment】
The specific embodiment for preparing the photovoltaic material of lamelliform perovskite structure is as follows：
1）The preparation of derivant solution
Cationic surfactant is configured to solution, its a concentration of CMC value of the solution using solvent deionized water
200%~300% to get to derivant solution；
2）The synthesis of presoma
The derivant solution is warming up to 30~40 DEG C, keeps the temperature, it is molten to the derivant under stirring
Halogenation methylamine organic solution is slowly added dropwise in liquid, fast drop lead halide organic solution, the two obtain after mixing again thereafter
The mixed liquor is warming up to 70~90 DEG C, stops stirring, 5~10min stood, thereafter using 2~5 DEG C/min's by mixed liquor
The mixed liquor is cooled to 30~40 DEG C by rate of temperature fall, and it is 10 to add in pH adjusting agent to adjust its pH value into the mixed liquor
Precursor solution is obtained after~14,20~30min of gentle agitation；
3）Crystal cures
The precursor solution is stood into 24~48h at room temperature, is followed by filtered, obtained solid is carried out a large amount of
It is secondary or water rinses three times, it is dried thereafter to get to the photovoltaic material of the lamelliform perovskite structure.
Cationic surfactant described in above-mentioned preparation process is preferably aliphatic ammonium salt, further preferably dodecyl
Trimethylammonium bromide（DTAB）, dodecyl trimethyl ammonium chloride（DTAC）, tetradecyltrimethylammonium bromide（TTAB）, 14
Alkyl trimethyl ammonium chloride（TTAC）, cetyl trimethylammonium bromide（CTAB）, hexadecyltrimethylammonium chloride（CTAC）
In it is one or more；Above-mentioned cationic active agent directly can bought or voluntarily prepare high-purity finished product on the market,
The methods of CMC value can obtain or be further advanced by electrical conductivity method, surface tension method, colorimetric method by inquiry is measured.
The preferred CH of halogenation methylamine3NH3I 、CH3NH3Br、 CH3NH3One or more in Cl, organic solution is
CH3NH3I 、CH3NH3Br、 CH3NH3One or more solution being dissolved in formed in organic solvent in Cl, it is described organic molten
Agent is preferably gamma-butyrolacton or DMF, and concentration is preferably 1.0~1.5mol/L.
The preferred PbCl of lead halide2、PbBr2、PbI2In one or more, organic solution PbCl2、PbBr2、
PbI2In one or more solution being dissolved in formed in organic solvent, the organic solvent is preferably gamma-butyrolacton or N,
Dinethylformamide（DMF）, concentration is preferably 1.0~1.5mol/L.
It is one or more in the preferred sodium hydroxide of the pH adjusting agent, potassium hydroxide, sodium bicarbonate.
Above-mentioned raw materials, solvent or conditioning agent can buy high purity product on the market（It analyzes pure or chemical pure）, also may be used
Voluntarily prepare high-purity finished product.
Solar cell assembles：
The preferable following manner group of the photovoltaic material of lamelliform perovskite structure being prepared by above-mentioned preparation method
Dress up solar cell：
1）According to FTO substrate of glass, TiO2Compacted zone, the photovoltaic material of lamelliform perovskite structure of the invention, conduction
The sequence to electrode of carbon material adds above-mentioned material and assembles to obtain solar cell successively；
2）In TiO2Porous support, such as TiO can be added between the photovoltaic material of compacted zone and lamelliform perovskite structure2/
Al2O3Composite bed in the photovoltaic material of lamelliform perovskite structure and can add between electrode spiro-OMeTAD hole transports
Layer；
3）When actually preparing, the thickness of the photovoltaic material of lamelliform perovskite structure is preferably 10 in the solar cell
~100nm.
With reference to the embodiment of the present invention, the invention will be further elaborated, detailed description below,
The above of the present invention is described in further detail again.But this should not be interpreted as to the range of the above-mentioned theme of the present invention only
It is limited to following example.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and usual
The various replacements or change that means are made, should all be included within the scope of the invention.
Embodiment 1
By dodecyl trimethyl ammonium bromide（DTAB）The molten of a concentration of 36mmol/L is configured to using solvent deionized water
The DTAB solution is warming up to 30 DEG C, keeps the temperature, is slowly added dropwise under stirring into the DTAB solution by liquid
CH3NH3The gamma-butyrolacton solution of I, CH in the solution3NH3The concentration of I is formulated as 1.5mol/L, after completion of dropwise addition again quickly to
PbI is wherein added dropwise2Gamma-butyrolacton solution, PbI in the solution2Concentration be formulated as 1.5mol/L, persistently stirred after completion of dropwise addition
It mixes to the two and is uniformly mixed, stop stirring after mixed liquor is warming up to 70 DEG C, 5min is stood, thereafter using the cooling of 2 DEG C/min
Mixed liquor is cooled to 30 DEG C by rate, and sodium hydroxide is added in into the mixed liquor and adjusts mixed liquor pH value to 10, is slowly stirred thereafter
It mixes mixed liquor 20min and obtains precursor solution, precursor solution standing is filtered afterwards for 24 hours at room temperature, by what is filtered
Solid is rinsed using a large amount of secondary water, is dried in baking oven after flushing to get to the lamelliform perovskite structure
Photovoltaic material, observe in the secure execution mode (sem the photovoltaic material be lamelliform crystal.
Embodiment 2
By tetradecyltrimethylammonium bromide（TTAB）The molten of a concentration of 8mmol/L is configured to using solvent deionized water
The TTAB solution is warming up to 35 DEG C, keeps the temperature, is slowly added dropwise under stirring into the TTAB solution by liquid
CH3NH3The gamma-butyrolacton solution of Cl, CH in the solution3NH3A concentration of 1.2mol/L of Cl, again quickly to it after completion of dropwise addition
Middle dropwise addition PbCl2Gamma-butyrolacton solution, PbCl in the solution2A concentration of 1.2mol/L, continued stirring until after completion of dropwise addition
The two is uniformly mixed, and stops stirring after mixed liquor is warming up to 80 DEG C, 7min is stood, thereafter using the rate of temperature fall of 3 DEG C/min
Mixed liquor is cooled to 40 DEG C, potassium hydroxide is added in into the mixed liquor and adjusts mixed liquor pH value to 12, is slowly stirred thereafter mixed
It closes liquid 25min and obtains precursor solution, be filtered after which is stood 48h at room temperature, the solid that will be filtered
It is rinsed, is dried in baking oven after flushing to get to the light of the lamelliform perovskite structure using a large amount of secondary water
Material is lied prostrate, the photovoltaic material is observed in the secure execution mode (sem as lamelliform crystal, per layer thickness slightly larger than the photovoltaic obtained in embodiment 1
Every layer thickness of material crystals.
Embodiment 3
By cetyl trimethylammonium bromide（CTAB）The molten of a concentration of 2.5mmol/L is configured to using solvent deionized water
The TTAB solution is warming up to 40 DEG C, keeps the temperature, is slowly added dropwise under stirring into the CTAB solution by liquid
CH3NH3The DMF solution of Br, CH in the solution3NH3The concentration of Br is formulated as 1.0mol/L, after completion of dropwise addition again it is quick thereto
PbBr is added dropwise2DMF solution, PbBr in the solution2Concentration be formulated as 1.0mol/L, both continued stirring until after completion of dropwise addition
It is uniformly mixed, stops stirring after mixed liquor is warming up to 70 DEG C, stand 8min, it thereafter will be mixed using the rate of temperature fall of 5 DEG C/min
It closes liquid and is cooled to 40 DEG C, sodium hydroxide and sodium bicarbonate adjusting mixed liquor pH value to 14 are added in into the mixed liquor, thereafter slowly
It is stirred liquid 30min and obtains precursor solution, be filtered, will filter after which is stood 48h at room temperature
Solid rinsed using a large amount of secondary water, be dried in baking oven after flushing to get to the lamelliform perovskite knot
The photovoltaic material of structure, observes the photovoltaic material as lamelliform crystal in the secure execution mode (sem, is slightly larger than in embodiment 2 per layer thickness and obtains
Photovoltaic material crystal every layer thickness.
Embodiment 4
By dodecyl trimethyl ammonium chloride（DTAC）The molten of a concentration of 40mmol/L is configured to using solvent deionized water
The DTAC solution is warming up to 40 DEG C, keeps the temperature, is slowly added dropwise under stirring into the DTAC solution by liquid
CH3NH3The DMF solution of Br, CH in the solution3NH3The concentration of Br is formulated as 1.0mol/L, after completion of dropwise addition again it is quick thereto
PbCl is added dropwise2DMF solution, PbCl in the solution2Concentration be formulated as 1.0mol/L, both continued stirring until after completion of dropwise addition
It is uniformly mixed, stops stirring after mixed liquor is warming up to 80 DEG C, stand 10min, it thereafter will be mixed using the rate of temperature fall of 4 DEG C/min
It closes liquid and is cooled to 40 DEG C, sodium hydroxide is added in into the mixed liquor and adjusts mixed liquor pH value to 13, is slowly stirred mixed liquor thereafter
25min obtains precursor solution, is filtered after which is stood 48h at room temperature, and the solid filtered is used
A large amount of secondary water is rinsed, and is dried in baking oven after flushing to get to the photovoltaic material of the lamelliform perovskite structure
Material observes the photovoltaic material as lamelliform crystal, per layer thickness slightly larger than the photovoltaic material obtained in embodiment 1 in the secure execution mode (sem
Every layer thickness of crystal is slightly less than every layer thickness of the photovoltaic material crystal obtained in embodiment 2.
Embodiment 5
By hexadecyltrimethylammonium chloride（CTAC）The molten of a concentration of 2.0mmol/L is configured to using solvent deionized water
The CTAC solution is warming up to 30 DEG C, keeps the temperature, is slowly added dropwise under stirring into the CTAC solution by liquid
CH3NH3The DMF solution of Cl, CH in the solution3NH3The concentration of Cl is formulated as 1.5mol/L, after completion of dropwise addition again it is quick thereto
PbI is added dropwise2DMF solution, PbI in the solution2Concentration be formulated as 1.5mol/L, both continued stirring until after completion of dropwise addition mixed
Uniform, stopping stirring after mixed liquor is warming up to 75 DEG C is closed, standing 10min will be mixed thereafter using the rate of temperature fall of 5 DEG C/min
Liquid is cooled to 30 DEG C, and sodium hydroxide is added in into the mixed liquor and adjusts mixed liquor pH value to 12, is slowly stirred mixed liquor thereafter
30min obtains precursor solution, is filtered after which is stood 48h at room temperature, and the solid filtered is used
A large amount of secondary water is rinsed, and is dried in baking oven after flushing to get to the photovoltaic material of the lamelliform perovskite structure
Material observes the photovoltaic material as lamelliform crystal, per layer thickness slightly larger than the photovoltaic material obtained in embodiment 3 in the secure execution mode (sem
Every layer thickness of crystal.
Embodiment 6
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass, the densification after heating 20min at 500 DEG C
Layer thickness is 50nm, thereafter dissolves the photovoltaic material of the lamelliform perovskite structure as made from embodiment 1 using DMF,
Thereafter it is spun on compacted zone, and the coating that the photovoltaic material is made to form 10nm for 10 minutes is heated at 90 DEG C and is affixed on compacted zone
Light-absorption layer is formed, then electrode slurry will be printed on by silk screen print method on the light-absorption layer, levelling is placed in 80 DEG C of baking ovens
Dry 10min obtains solar cell, its photoelectric conversion efficiency is 13% after tested, current density 24.0mA/cm2, open circuit
Voltage 893mV.
Embodiment 7
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass, the densification after heating 25min at 500 DEG C
Layer thickness is 40nm, thereafter dissolves the photovoltaic material of the lamelliform perovskite structure as made from embodiment 2 using DMF,
Thereafter it is spun on compacted zone, and the coating that the photovoltaic material is made to form 20nm for 10 minutes is heated at 80 DEG C and is affixed on compacted zone
Light-absorption layer is formed, then electrode slurry will be printed on by silk screen print method on the light-absorption layer, levelling is placed in 80 DEG C of baking ovens
Dry 10min obtains solar cell, its photoelectric conversion efficiency is 12.3% after tested, current density 20.0mA/cm2, open
Road voltage 912mV.
Embodiment 8
One block of FTO glass is selected, is cleaned up and is further dried, screen printing is used on the backward FTO glass
Brush method prints one layer of TiO2Film layer obtains the compacted zone being carried on FTO glass, the densification after heating 25min at 500 DEG C
Layer thickness is 50nm, thereafter dissolves the photovoltaic material of the lamelliform perovskite structure as made from embodiment 3 using DMF,
Thereafter it is spun on compacted zone, and the coating that the photovoltaic material is made to form 30nm for 10 minutes is heated at 80 DEG C and is affixed on compacted zone
Light-absorption layer is formed, then electrode slurry will be printed on by silk screen print method on the light-absorption layer, levelling is placed in 80 DEG C of baking ovens
Dry 10min obtains solar cell, its photoelectric conversion efficiency is 10% after tested, current density 18.2mA/cm2, open circuit
Voltage 930mV.
Claims (8)
1. a kind of preparation method of the photovoltaic material of lamelliform perovskite structure, it is characterised in that：Include the following steps：
1）The preparation of derivant solution
Cationic surfactant is configured to solution, a concentration of cationic surface of the solution using solvent deionized water
The 200%~300% of the CMC value of activating agent is to get to derivant solution；The cationic surfactant is selected from dodecyl
Trimethylammonium bromide, dodecyl trimethyl ammonium chloride, tetradecyltrimethylammonium bromide, tetradecyl trimethyl ammonium chloride,
It is one or more in cetyl trimethylammonium bromide, hexadecyltrimethylammonium chloride；
2）The synthesis of presoma
The derivant solution is warming up to 30~40 DEG C, keeps the temperature, under stirring into the derivant solution
Halogenation methylamine organic solution is slowly added dropwise, fast drop lead halide organic solution, the two are mixed after mixing again thereafter
The mixed liquor is warming up to 70~90 DEG C, stops stirring, 5~10min stood, thereafter using the cooling of 2~5 DEG C/min by liquid
The mixed liquor is cooled to 30~40 DEG C by rate, and add in into the mixed liquor pH adjusting agent adjust its pH value for 10~
Precursor solution is obtained after 14,20~30min of gentle agitation；
3）Crystal cures
The precursor solution is stood into 24~48h at room temperature, is followed by filtered, obtained solid is carried out a large amount of two
It is secondary or water rinses three times, it is dried thereafter to get to the photovoltaic material of the lamelliform perovskite structure.
2. the preparation method of the photovoltaic material of lamelliform perovskite structure according to claim 1, it is characterised in that：It is described
Halogenation methylamine is one or more in CH3NH3I, CH3NH3Br, CH3NH3Cl.
3. the preparation method of the photovoltaic material of lamelliform perovskite structure according to claim 1, it is characterised in that：It is described
Halogenation methylamine organic solution is dissolved in institute's shape in organic solvent for one or more in CH3NH3I, CH3NH3Br, CH3NH3Cl
Into solution, the organic solvent be gamma-butyrolacton or DMF.
4. the preparation method of the photovoltaic material of lamelliform perovskite structure according to claim 1, it is characterised in that：It is described
Lead halide is one or more in PbCl2, PbBr2, PbI2.
5. the preparation method of the photovoltaic material of lamelliform perovskite structure according to claim 1, it is characterised in that：It is described
Lead halide organic solution is one or more solution being dissolved in formed in organic solvent in PbCl2, PbBr2, PbI2, described
Organic solvent be gamma-butyrolacton or N, dinethylformamide（DMF）.
6. the preparation method of the photovoltaic material of lamelliform perovskite structure according to claim 1, it is characterised in that：It is described
PH adjusting agent is one or more in sodium hydroxide, potassium hydroxide, sodium bicarbonate.
7. the preparation method of the photovoltaic material of lamelliform perovskite structure according to claim 1, it is characterised in that：It is described
The .5mol/L of a concentration of 1 .0 of lead halide in halogenation methylamine organic solution~1；Lead halide in the lead halide organic solution
The .5mol/L of a concentration of 1 .0~1.
8. a kind of photovoltaic material of lamelliform perovskite structure, it is characterised in that：It passes through described in any one of claim 1~7
Preparation method be prepared, crystal be lamelliform.
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| CN106025067B (en) * | 2016-07-30 | 2019-06-18 | 哈尔滨工业大学深圳研究生院 | A kind of solwution method generates film build method and its device application of perovskite thin film |
| CN107722962B (en) * | 2016-08-12 | 2019-09-17 | 京东方科技集团股份有限公司 | Luminescent material and preparation method thereof, nanometer sheet membrane material, backlight and display device |
| KR101894413B1 (en) * | 2017-04-04 | 2018-09-04 | 성균관대학교산학협력단 | Fabrication method of a solar cell |
| CN109148687B (en) * | 2017-06-16 | 2023-02-07 | 韩国化学研究院 | Perovskite solar cell including wide band gap and method for manufacturing same |
| CN108539026B (en) * | 2018-05-03 | 2021-06-25 | 河南科技大学 | Preparation method of perovskite thin film with micron tube array structure |
| CN109065725A (en) * | 2018-07-19 | 2018-12-21 | 陕西师范大学 | A method of the perovskite solar battery that surfactant prepares efficient stable being added in calcium titanium ore bed |
| CN110880554B (en) * | 2018-09-05 | 2023-04-07 | 杭州纤纳光电科技有限公司 | Equipment and method for coating precursor solution and surfactant step by step |
| CN110880550A (en) * | 2018-09-05 | 2020-03-13 | 杭州纤纳光电科技有限公司 | Coating equipment and method for precursor solution containing surfactant |
| CN110880555A (en) * | 2018-09-05 | 2020-03-13 | 杭州纤纳光电科技有限公司 | Coating equipment and method for mixed solution of precursor and surfactant |
| CN110880551A (en) * | 2018-09-05 | 2020-03-13 | 杭州纤纳光电科技有限公司 | Perovskite solution coating equipment containing surfactant and method thereof |
| CN109545972B (en) * | 2018-11-23 | 2022-12-02 | 浙江昱辉阳光能源江苏有限公司 | High-stability perovskite solar cell and preparation method |
| CN111710784B (en) * | 2020-06-18 | 2023-04-07 | 浙江浙能技术研究院有限公司 | Perovskite suspension state precursor liquid and film forming method |
| CN113823740A (en) * | 2021-08-05 | 2021-12-21 | 中国科学院深圳先进技术研究院 | Perovskite-based X-ray detector with n-i structure and preparation method thereof |
| CN118109906A (en) * | 2024-03-04 | 2024-05-31 | 天津大学 | Preparation method, product and application of perovskite microcrystal |
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