CN106917064A - Single step original position flash method growth ABX3The preparation method of type perovskite thin film - Google Patents
Single step original position flash method growth ABX3The preparation method of type perovskite thin film Download PDFInfo
- Publication number
- CN106917064A CN106917064A CN201710082345.XA CN201710082345A CN106917064A CN 106917064 A CN106917064 A CN 106917064A CN 201710082345 A CN201710082345 A CN 201710082345A CN 106917064 A CN106917064 A CN 106917064A
- Authority
- CN
- China
- Prior art keywords
- perovskite
- thin film
- substrate
- abx
- perovskite thin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/243—Crucibles for source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5806—Thermal treatment
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/16—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering
- H10K71/164—Deposition of organic active material using physical vapour deposition [PVD], e.g. vacuum deposition or sputtering using vacuum deposition
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of single step original position flash method growth ABX3The preparation method of type perovskite thin film, is applied to new material manufacturing process area.Perovskite thin film preparation method is as follows：Single evaporation source is done with the solution of perovskite material, heater is added on substrate, after treating that vacuum reaches certain requirement, under conditions of sample substrate temperature is uniform temperature, quickly electric current is added to rapidly using moment is not less than 200A, evaporator temperature moment is reached the temperature for being not less than 1000 DEG C, the distillation of material moment, after annealing is directly finally carried out in vacuum cavity, the ABX for being stablized3Type perovskite thin film.The perovskite thin film that the present invention is prepared using single step original position flash method, energy consumption is low, and evaporation rate is fast, and the time is short, and film is without cavity and large area is uniform, and substrate range of choice is wide, is adapted to do planar device.
Description
Technical field
The present invention relates to a kind of preparation method of perovskite thin film, more particularly to one kind prepares calcium titanium by depositing operation
The method of ore deposit film, is applied to photoelectric device preparing technical field.
Background technology
Today's society, the development of the mankind is increasingly rapid, and the development of human society then be unable to do without the energy.For a long time, people
The main energy sources that class is utilized have the non-renewable energy resources such as coal, oil and natural gas.Since 21 century, as people produce
The rapid raising of life, demand and consumption to the energy also significantly increase, and non-renewable energy resources are faced with the crisis of exhaustion,
Therefore new, clean regenerative resource is found as the task of top priority.There are various new energy to be constantly utilized exploitation at present, such as too
Positive energy, water energy, wind energy etc..Wherein solar energy due to its originate innumerable and stability, as most development potentiality can
Renewable new energy source.Formula currently with solar energy mainly has two kinds：Photothermal deformation and opto-electronic conversion.Photothermal conversion is extensive
Using its topmost representative is exactly solar water heater；And photoelectric conversion is then in high speed development stage, its best side
Formula is exactly solar cell, is also called photovoltaic cell.Solar cell pollution-free, zero-emission, is not produced during photoelectric conversion
Any noise of life and radiation, are a kind of excellent reforming units of environment-friendly green energy resource.
Crystal silicon solar energy battery is still occupied an leading position in current photovoltaic market, and efficiency is close to 20%.But monocrystalline silicon
Time consumption and energy consumption.Although second generation solar cell saves material, growth cost is low, also there is a unavoidable shortcoming, Te,
In, Ga etc. are the little elements of reserves on the earth, more rare than Au, and this will be such that it cannot mass produces, strong influence
Its output value.Third generation solar cell, such as organic photovoltaic (OPVs), DSSC (DSCs) and quantum dot
Solar cell (QDSCs), is that, by blade coating, the technique such as Shiscreen printings and spraying is coated in unconventional substrate by solution
So as to ensure low-cost solar cell power generation.Recently, a kind of fast development of new material has attracted industrial circle and many to grind
The attention of the person of studying carefully.CH with perovskite structure3NH3PbX3Material, wherein X=I, Br, Cl, are that a kind of energy gap is 1.5eV
Direct band gap material.It is risen violently rapidly in recent years with the conversion efficiency of the solar cell that it is main absorbing layer,
3.8% from the beginning has broken through to 20.1%, becomes the study hotspot of domestic and international photovoltaic art.The preparation method of the material
Predominantly chemical method.Such as spin-coating method and the two-step method based on spin-coating method.Both approaches all can be based on porous material
TiO2With high-quality film is deposited in ZnO, so as to obtain high efficiency.But due to film out-of-flatness prepared by spin-coating method, cover
Lid rate is not high, and this will reduce the absorption of photon, and reduce parallel resistance simultaneously, reduce device efficiency, for planar device
Unsuitable, on the other side to be, the method based on vacuum can obviously improve film coverage.What such as professor Snaith used is double
The method of steaming substantially improves deficiency of the film of spin-coating method preparation on coverage rate, thickness evenness and pore quantity altogether in source, is formed
Continuous film, its crystallite dimension is in micron dimension.But double source method control is complicated, two independent evaporation sources need control to exist
Certain temperature range, is that evaporation rate can be stablized it is determined that in ratio.In addition, to realize high-quality thin film, evaporation rate is needed
It is very slow, generally require control it is per second at 0.5 angstrom within, so low speed is not suitable for large-scale production.
The content of the invention
In order to solve prior art problem, it is an object of the invention to overcome the shortcomings of that prior art is present, there is provided a kind of
Single step original position flash method growth ABX3The preparation method of type perovskite thin film, is done using the solution or powder of perovskite material and evaporated
Source, directly prepares perovskite thin film, as the absorbed layer of solar cell, to prepare high conversion efficiency with single step original position flash method
Perovskite thin film solar cell a kind of new technique is provided.
Purpose is created to reach foregoing invention, the present invention uses following technical proposals：
A kind of single step original position flash method growth ABX3The preparation method of type perovskite thin film, comprises the following steps：
A. substrate pre-treatment：
Substrate uses FTO substrates, ITO substrates or Si substrates, and pre-treatment step is：
By FTO substrates or ITO substrate transparent conducting glass substrate first using the logical cleaning substrate surface of Qula, then spend from
Sub- water cleaning, is respectively adopted acetone, EtOH Sonicate and cleans at least 15 minutes, then with deionized water rinsing electrically conducting transparent glass afterwards
Glass substrate surface, is then dried to transparent conducting glass substrate, finally using the treatment of ultraviolet combined with ozone or microwave etc.
Gas ions process transparent conducting glass substrate surface, obtain the transparent conducting glass substrate of cleaning；Or by Si substrates spend from
Sub- water cleaning, is then not less than 98% concentrated sulfuric acid immersion Si substrates using mass percent concentration, then takes out Si substrates, then
Remaining sulfuric acid on removal Si substrates is cleaned using deionized water, then Si substrates are dried, finally combined using ultraviolet
Ozone treatment or Microwave plasma treatment Si substrate surfaces, obtain the silicon substrate of cleaning；
B. single step is in situ flashes perovskite thin film：
Using into perovskite solution or perovskite powders, being prepared into perovskite solution or perovskite powders, perovskite solution
Or perovskite powders are ABX3Type organic inorganic hybridization perovskite material, wherein A is positive monovalence organic molecule group, and B is just
Divalent metal element, X is negative one valency halogen；Evaporation of metal boat is pre-processed, evaporation of metal boat be tantalum piece, molybdenum sheet or
Leaf；Perovskite solution or perovskite powders are uniformly laid on evaporation of metal boat, then vaporization chamber air pressure is vacuumized
To less than 2 × 10-2Pa, under conditions of the underlayer temperature pre-processed by the step a is design temperature, is added to substrate
The current control of heat is not higher than 1.6A, applies big using the quick heater in vaporization chamber of moment in the time of not higher than 1 second
Electric current, and the electric current applied to heater is added to rapidly be not less than 200A, reach the temperature moment of evaporation boat and be not less than
1000 DEG C, make the perovskite solution on evaporation boat or perovskite powders material transient evaporation or distillation, by rapid evaporation technique
Perovskite thin film is deposited to substrate surface, whole flash evaporation processes are no more than 5 seconds, finally in vaporization chamber prepared by flash process
Perovskite thin film carry out after annealing, and apply electric current to the heater of control annealing temperature in annealing and be not higher than 2A, obtain final product
To the ABX of stabilization3Type perovskite thin film.
As currently preferred technical scheme, in the step b, using into perovskite solution or perovskite powders,
Perovskite solution or perovskite powders are prepared into, perovskite solution or perovskite powders are FAPbX3Organic inorganic hybridization perovskite
Material, wherein A are positive monovalence organic molecule groups, and X is negative one valency halogen.
As the further preferred technical scheme of such scheme, in the step b, using into perovskite solution or calcium
Titanium ore powder, is prepared into perovskite solution or perovskite powders, and perovskite solution or perovskite powders are CH3NH3PbX3Organic nothing
Machine hydridization perovskite material, wherein X is negative one valency halogen.
As the further preferred technical scheme of such scheme, in the step b, using into perovskite solution or calcium
Titanium ore powder, is prepared into perovskite solution or perovskite powders, and perovskite solution or perovskite powders are to include CH3NH3PbX3With
FAPbX3ABX3Type organic inorganic hybridization perovskite material, wherein A is positive monovalence organic molecule group, and X is negative one valency halogen family
Element.
As the further preferred technical scheme of such scheme, in the step b, after substrate pre-treatment, and right
Substrate carries out flash process deposition and prepares ABX3Before type perovskite thin film, one layer of electron transfer layer is prepared also on substrate
PCBM, after carrying out flash process, i.e., forms ABX on the electron transfer layer PCBM combined with substrate3Type perovskite thin film.
Used as the further preferred technical scheme of such scheme, in the step b, X is any one in I, Br and Cl
Plant halogen or any several halogens are combined.
The present invention compared with prior art, substantive distinguishing features and remarkable advantage is obviously protruded with following：
1. the present invention is a kind of physical growth method of fast growth simple to operate, i.e., single step original position flash method prepares organic
Inorganic hybridization perovskite thin film material, the inventive method process is simple, it is easy to operate, favorable repeatability, organic inorganic hybridization calcium
Titanium ore thin-film material；
2. the present invention is processed relative to re-annealing after the general solution spin coating of prior art and is advantageous in that, can growth in situ
Go out the FAPbI of pure Emission in Cubic3Perovskite thin film, it is good with thin film crystallization quality, the characteristics of perovskite thin film surfacing；
3. the perovskite thin film that the present invention is prepared using single step original position flash method, energy consumption is low, and evaporation rate is fast, and the time is short,
Film is without cavity and large area is uniform, and substrate range of choice is wide, is adapted to prepare planar device.
Brief description of the drawings
Fig. 1 is the apparatus structure principle schematic of the single step of the embodiment of the present invention one original position flash method.
Fig. 2 is the single step of the embodiment of the present invention one original position flash method growth FAPbI3The X-ray diffractogram of perovskite thin film.
Fig. 3 is the single step of the embodiment of the present invention one original position flash method growth FAPbI3The SEM of perovskite thin film
Figure.
Specific embodiment
Details are as follows for the preferred embodiments of the present invention：
Embodiment one：
In the present embodiment, referring to Fig. 1, a kind of single step original position flash method growth FAPbI3The preparation side of perovskite thin film
Method, comprises the following steps：
A. substrate pre-treatment：
Using the SnO for mixing F2FTO, by transparent conducting glass SnO2:F is as deposition substrate, pre-treatment step：
FTO transparent conducting glass substrate etchings are first gone out into required pattern, then deionized water punching with zinc powder and watery hydrochloric acid
Wash clean, then first removes the spot of substrate surface using the logical cleaning substrate surface of Qula, is then cleaned with deionized water, will
The remaining Qula of substrate surface is logical to be rinsed out, and acetone, EtOH Sonicate is respectively adopted afterwards and cleans 15 minutes, then uses deionized water
FTO transparent conducting glass substrate surfaces are rinsed, then FTO transparent conducting glass substrates is dried, finally using ultraviolet
Combined with ozone treatment surface 10 minutes, obtains the FTO transparent conducting glass substrates of cleaning；
Then 5mg PCBM are taken to be dissolved in the chlorobenzene of 1ml, 12h is stirred at room temperature, be allowed to be sufficiently mixed, under dark condition,
Spin coating electron transfer layer PCBM on pretreated FTO transparent conducting glass substrate, spin coating parameters are 50ul, 4000rpm/20s,
Annealed 20 minutes at 70 DEG C, obtain combining the substrate of electron transfer layer PCBM；
B. single step is in situ flashes perovskite thin film：
Weigh certain mass than PbI2With FAI powder, two kinds of different powder are dissolved in organic solvent, are made into one
Determine the FAPbI of mol ratio3Perovskite solution, 50 DEG C and heating stirring 12h of insulation, evaporation of metal boat is pre-processed, metal
Evaporation boat uses molybdenum sheet, by FAPbI3Perovskite solution is uniformly applied on evaporation of metal boat, is then taken out vaporization chamber air pressure
Vacuum is to less than 2 × 10-2Pa, continues to keep pumping speed to keep this vacuum, the combination electron transfer layer in the step a
The substrate temperature of PCBM is under conditions of design temperature, the current control for as being heated to substrate is the condition of 1.6A
Under, high current is applied using the quick heater in vaporization chamber of moment in the time of not higher than 1 second, and will apply to heater
Electric current add to 200A rapidly, the temperature moment of evaporation boat is reached 1000 DEG C, make the perovskite solution liquid film wink on evaporation boat
Between gasify, by rapid evaporation technique to substrate surface deposit perovskite thin film, whole flash evaporation processes be less than 5 seconds, finally
After annealing is carried out to perovskite thin film prepared by flash process in vaporization chamber, and in annealing to the heater of control annealing temperature
It is 2A to apply electric current, that is, the FAPbI for being stablized3Perovskite thin film.
The solution of the present embodiment perovskite material does single evaporation source, and heater is added on substrate, treats vacuum
Reach after certain requirement, under conditions of sample substrate temperature is uniform temperature, quickly added to electric current rapidly using moment
200A, makes evaporator temperature moment reach 1000 DEG C, and the evaporation of material transient evaporation is finally directly retreated in vacuum cavity
Fire, the FAPbI3 perovskite thin films stablized.
Experimental test and analysis：
Referring to organic inorganic hybridization FAPbI prepared by Fig. 2 and Fig. 3, embodiment one3Perovskite thin film crystalline quality is good, calcium
Titanium ore film surface is smooth, and process repeatability is good, the perovskite thin film that embodiment one is prepared using single step original position flash method, energy
Consumption is low, and evaporation rate is fast, and the time is short, and film is without cavity and large area is uniform, and substrate range of choice is wide, is adapted to prepare plane device
Part.
Embodiment two：
The present embodiment is essentially identical with embodiment one, is particular in that：
In the present embodiment, a kind of single step original position flash method growth FAPbI3The preparation method of perovskite thin film, including such as
Lower step：
A. substrate pre-treatment：
Using Si substrates, using Si substrates as deposition substrate, pre-treatment step is：
Si substrates are cleaned with deionized water, then uses mass percent concentration to soak Si bases for 98.3% concentrated sulfuric acid
Piece, then takes out Si substrates, reuses remaining sulfuric acid on deionized water cleaning removal Si substrates, and then Si substrates are done
It is dry, finally using Microwave plasma treatment Si substrate surfaces 10 minutes, obtain the silicon substrate of cleaning；
Then 5mg PCBM are taken to be dissolved in the chlorobenzene of 1ml, 12h is stirred at room temperature, be allowed to be sufficiently mixed, under dark condition,
Spin coating electron transfer layer PCBM in pretreated Si base substrates, spin coating parameters are 50ul, 4000rpm/20s, at 70 DEG C
Annealing 20 minutes, obtains combining the substrate of electron transfer layer PCBM；
B. single step is in situ flashes perovskite thin film：
Weigh certain mass than PbI2And FAI, uniformly it is mixed and made into FAPbI3Perovskite powders, evaporation of metal boat is entered
Row pretreatment, evaporation of metal boat uses molybdenum sheet, by FAPbI3Perovskite powders are uniformly laid on evaporation of metal boat, then will
Vaporization chamber air pressure is evacuated to less than 2 × 10-2Pa, closes vavuum pump or valve, the combination electron transfer layer in the step a
The substrate temperature of PCBM is under conditions of design temperature, the current control for as being heated to substrate is the condition of 1.6A
Under, high current is applied using the quick heater in vaporization chamber of moment in the time of not higher than 1 second, and will apply to heater
Electric current add to 200A rapidly, the temperature moment of evaporation boat is reached 1000 DEG C, make the FAPbI on evaporation boat3Perovskite powders
Material moment is distilled, and perovskite thin film is deposited to substrate surface by rapid evaporation technique, and whole flash evaporation processes are less than 5
Second, after annealing is finally carried out to perovskite thin film prepared by flash process in vaporization chamber, and in annealing to control annealing temperature
Heater apply electric current be 2A, that is, the FAPbI for being stablized3Perovskite thin film.
The solution of the present embodiment perovskite material does single evaporation source, and heater is added on substrate, treats vacuum
Reach after certain requirement, under conditions of sample substrate temperature is uniform temperature, quickly added to electric current rapidly using moment
200A, makes evaporator temperature moment reach 1000 DEG C, and the distillation of material moment finally directly carries out after annealing in vacuum cavity,
The FAPbI3 perovskite thin films stablized.The perovskite thin film prepared using single step original position flash method has energy consumption low, evaporates
Speed is fast, and the time is short, and film is without cavity and large area is uniform, and substrate range of choice is wide, is adapted to the characteristics of doing planar device.
The embodiment of the present invention is illustrated above in conjunction with accompanying drawing, but the invention is not restricted to above-described embodiment, can be with
The purpose of innovation and creation of the invention makes various changes, under all Spirit Essence and principle according to technical solution of the present invention
Change, modification, replacement, the combination or simplified made, should be equivalent substitute mode, as long as meeting goal of the invention of the invention,
Without departing from single step of the present invention original position flash method growth ABX3The know-why of the preparation method of type perovskite thin film and invention
Design, belongs to protection scope of the present invention.
Claims (6)
1. a kind of single step original position flash method grows ABX3The preparation method of type perovskite thin film, it is characterised in that including following step
Suddenly：
A. substrate pre-treatment：
Substrate uses FTO substrates, ITO substrates or Si substrates, and pre-treatment step is：
By FTO substrates or ITO substrate transparent conducting glass substrate first using the logical cleaning substrate surface of Qula, deionized water is then used
Cleaning, is respectively adopted acetone, EtOH Sonicate and cleans at least 15 minutes, then with deionized water transparent conducting glass substrate table afterwards
Face, is then dried to transparent conducting glass substrate, finally uses at the treatment of ultraviolet combined with ozone or microwave plasma
Reason transparent conducting glass substrate surface, obtains the transparent conducting glass substrate of cleaning；Or Si substrates are cleaned with deionized water,
Then using mass percent concentration be not less than 98% concentrated sulfuric acid immersion Si substrates, then by Si substrates take out, reuse from
Remaining sulfuric acid on sub- water cleaning removal Si substrates, is then dried, finally using the treatment of ultraviolet combined with ozone to Si substrates
Or Microwave plasma treatment Si substrate surfaces, obtain the silicon substrate of cleaning；
B. single step is in situ flashes perovskite thin film：
Using into perovskite solution or perovskite powders, perovskite solution or perovskite powders are ABX3Type organic inorganic hybridization calcium
Titanium ore material, wherein A are positive monovalence organic molecule groups, and B is positive divalent metal element, and X is negative one valency halogen；By gold
Category evaporation boat is pre-processed, and evaporation of metal boat is tantalum piece, molybdenum sheet or leaf；Perovskite solution or perovskite powders is uniform
It is laid on evaporation of metal boat, then vaporization chamber air pressure is evacuated to less than 2 × 10-2Pa, pre-processes by the step a
Underlayer temperature under conditions of design temperature, the current control heated to substrate not higher than 1.6A, using not higher than 1 second
Time in the moment quick heater in vaporization chamber apply high current, and the electric current applied to heater is added to not rapidly
Less than 200A, reach the temperature moment of evaporation boat and be not less than 1000 DEG C, make the perovskite solution or perovskite powder on evaporation boat
Powder material transient evaporation or distillation, perovskite thin film, whole flash process mistake are deposited by rapid evaporation technique to substrate surface
Journey is no more than 5 seconds, and after annealing is finally carried out to perovskite thin film prepared by flash process in vaporization chamber, and in annealing to control
The heater of annealing temperature applies electric current and is not higher than 2A, that is, the ABX for being stablized3Type perovskite thin film.
2. single step original position flash method grows ABX according to claim 13The preparation method of type perovskite thin film, its feature exists
In：In the step b, using into perovskite solution or perovskite powders, perovskite solution or perovskite powders, calcium are prepared into
Titanium ore solution or perovskite powders are FAPbX3Organic inorganic hybridization perovskite material, wherein A are positive monovalence organic molecule bases
Group, X is negative one valency halogen.
3. single step original position flash method grows ABX according to claim 23The preparation method of type perovskite thin film, its feature exists
In：In the step b, using into perovskite solution or perovskite powders, perovskite solution or perovskite powders, calcium are prepared into
Titanium ore solution or perovskite powders are CH3NH3PbX3Organic inorganic hybridization perovskite material, wherein X are negative one valency halogens.
4. single step original position flash method grows ABX according to claim 23The preparation method of type perovskite thin film, its feature exists
In：In the step b, using into perovskite solution or perovskite powders, perovskite solution or perovskite powders, calcium are prepared into
Titanium ore solution or perovskite powders are to include CH3NH3PbX3And FAPbX3ABX3Type organic inorganic hybridization perovskite material, wherein
A is positive monovalence organic molecule group, and X is negative one valency halogen.
5. single step original position flash method grows ABX according to any one in Claims 1 to 43The preparation side of type perovskite thin film
Method, it is characterised in that：In the step b, after substrate pre-treatment, and ABX is prepared flash process deposition is carried out to substrate3Type
Before perovskite thin film, one layer of electron transfer layer PCBM is prepared also on substrate, after carrying out flash process, i.e., combined with substrate
Electron transfer layer PCBM on form ABX3Type perovskite thin film.
6. single step original position flash method grows ABX according to any one in Claims 1 to 43The preparation side of type perovskite thin film
Method, it is characterised in that：In the step b, X is any one halogen or any several halogen knots in I, Br and Cl
Close.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710082345.XA CN106917064A (en) | 2017-02-16 | 2017-02-16 | Single step original position flash method growth ABX3The preparation method of type perovskite thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710082345.XA CN106917064A (en) | 2017-02-16 | 2017-02-16 | Single step original position flash method growth ABX3The preparation method of type perovskite thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106917064A true CN106917064A (en) | 2017-07-04 |
Family
ID=59453706
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710082345.XA Pending CN106917064A (en) | 2017-02-16 | 2017-02-16 | Single step original position flash method growth ABX3The preparation method of type perovskite thin film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106917064A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108447996A (en) * | 2018-02-07 | 2018-08-24 | 友达光电股份有限公司 | Perovskite structure, electronic device using same, and method for manufacturing photoelectric conversion layer |
| CN109216547A (en) * | 2018-09-20 | 2019-01-15 | 西安交通大学 | A kind of preparation method of perovskite thin film and its preparation method of solar battery |
| CN110047774A (en) * | 2018-01-17 | 2019-07-23 | 杭州纤纳光电科技有限公司 | A kind of immersion prepares the equipment and application method and application of perovskite thin film |
| CN110724934A (en) * | 2018-07-17 | 2020-01-24 | 杭州纤纳光电科技有限公司 | Powder evaporation device and using method and application thereof |
| CN111704159A (en) * | 2020-06-23 | 2020-09-25 | 西北工业大学 | Method for realizing type switching of lead-based perovskite nanosheets |
| CN113745438A (en) * | 2021-07-19 | 2021-12-03 | 暨南大学 | Large-area perovskite light-emitting film and light-emitting diode thereof |
| CN114314659A (en) * | 2021-12-30 | 2022-04-12 | 华中科技大学 | Two-dimensional inorganic molecular crystal Sb2O3Nano material, preparation method and application |
| CN115343266A (en) * | 2022-08-29 | 2022-11-15 | 北京交通大学 | Preparation method of lead ion fluorescence detection tool |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5350606A (en) * | 1989-03-30 | 1994-09-27 | Kanegafuchi Chemical Industry Co., Ltd. | Single crystal ferroelectric barium titanate films |
| CN104134720A (en) * | 2014-07-10 | 2014-11-05 | 上海大学 | Preparation method of organic and inorganic hybridization perovskite material growing by single-source flash evaporation method and plane solar cell of material |
| CN105239054A (en) * | 2015-11-03 | 2016-01-13 | 天津理工大学 | Preparation device and method for organic and inorganic hybrid perovskite film with micro grain size |
-
2017
- 2017-02-16 CN CN201710082345.XA patent/CN106917064A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5350606A (en) * | 1989-03-30 | 1994-09-27 | Kanegafuchi Chemical Industry Co., Ltd. | Single crystal ferroelectric barium titanate films |
| CN104134720A (en) * | 2014-07-10 | 2014-11-05 | 上海大学 | Preparation method of organic and inorganic hybridization perovskite material growing by single-source flash evaporation method and plane solar cell of material |
| CN105239054A (en) * | 2015-11-03 | 2016-01-13 | 天津理工大学 | Preparation device and method for organic and inorganic hybrid perovskite film with micro grain size |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7037838B2 (en) | 2018-01-17 | 2022-03-17 | 杭州繊納光電科技有限公司 | A vapor deposition device for manufacturing perovskite film, its usage, and a method for manufacturing perovskite solar cells. |
| CN110047774A (en) * | 2018-01-17 | 2019-07-23 | 杭州纤纳光电科技有限公司 | A kind of immersion prepares the equipment and application method and application of perovskite thin film |
| EP3723118A4 (en) * | 2018-01-17 | 2021-03-10 | Hangzhou Microquanta Semiconductor Corporation Limited | Apparatus for immersion-based preparation of perovskite thin film, use method and application thereof |
| CN110047774B (en) * | 2018-01-17 | 2021-08-27 | 杭州纤纳光电科技有限公司 | Equipment for preparing perovskite thin film in immersion mode, use method and application |
| JP2021507542A (en) * | 2018-01-17 | 2021-02-22 | 杭州繊納光電科技有限公司Ｈａｎｇｚｈｏｕ Ｍｉｃｒｏｑｕａｎｔａ Ｓｅｍｉｃｏｎｄｕｃｔｏｒ Ｃｏ．，Ｌｔｄ | Immersion device for producing perovskite film, usage and its use |
| KR20200100148A (en) * | 2018-01-17 | 2020-08-25 | 항조우 마이크로콴타 세미컨덕터 컴퍼니 리미티드 | Submerged manufacturing device of perovskite thin film and its usage and application |
| KR102418868B1 (en) | 2018-01-17 | 2022-07-07 | 항조우 마이크로콴타 세미컨덕터 컴퍼니 리미티드 | Immersion-type manufacturing device of perovskite thin film, usage method and application |
| JP7037838B6 (en) | 2018-01-17 | 2022-04-01 | 杭州繊納光電科技有限公司 | A vapor deposition device for manufacturing perovskite film, its usage, and a method for manufacturing perovskite solar cells. |
| WO2019141045A1 (en) * | 2018-01-17 | 2019-07-25 | 杭州纤纳光电科技有限公司 | Apparatus for immersion-based preparation of perovskite thin film, use method and application thereof |
| CN108447996A (en) * | 2018-02-07 | 2018-08-24 | 友达光电股份有限公司 | Perovskite structure, electronic device using same, and method for manufacturing photoelectric conversion layer |
| CN108447996B (en) * | 2018-02-07 | 2022-06-28 | 友达光电股份有限公司 | Perovskite structure, electronic device using same, and method for manufacturing related photoelectric conversion layer |
| CN110724934A (en) * | 2018-07-17 | 2020-01-24 | 杭州纤纳光电科技有限公司 | Powder evaporation device and using method and application thereof |
| CN109216547A (en) * | 2018-09-20 | 2019-01-15 | 西安交通大学 | A kind of preparation method of perovskite thin film and its preparation method of solar battery |
| CN109216547B (en) * | 2018-09-20 | 2020-08-28 | 西安交通大学 | Preparation method of perovskite thin film and preparation method of solar cell thereof |
| CN111704159A (en) * | 2020-06-23 | 2020-09-25 | 西北工业大学 | Method for realizing type switching of lead-based perovskite nanosheets |
| CN113745438A (en) * | 2021-07-19 | 2021-12-03 | 暨南大学 | Large-area perovskite light-emitting film and light-emitting diode thereof |
| CN114314659A (en) * | 2021-12-30 | 2022-04-12 | 华中科技大学 | Two-dimensional inorganic molecular crystal Sb2O3Nano material, preparation method and application |
| CN115343266A (en) * | 2022-08-29 | 2022-11-15 | 北京交通大学 | Preparation method of lead ion fluorescence detection tool |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106917064A (en) | Single step original position flash method growth ABX3The preparation method of type perovskite thin film | |
| CN104362253B (en) | All solid state perovskite microcrystalline silicon composite solar battery and preparation method thereof | |
| CN105609643B (en) | A kind of Ca-Ti ore type solar cell and preparation method | |
| CN108493340B (en) | Method for preparing perovskite solar cell with assistance of steam | |
| CN103700768A (en) | Perovskite structural solar battery and preparation method thereof | |
| CN104134720A (en) | Preparation method of organic and inorganic hybridization perovskite material growing by single-source flash evaporation method and plane solar cell of material | |
| CN111092160B (en) | Method for passivating lower interface of perovskite solar cell with inverse structure | |
| CN112331740B (en) | Preparation method of inorganic perovskite solar cell adopting spin coating-evaporation two-step method | |
| CN106953014B (en) | Hybrid solar cell structure with copper phthalocyanine as hole transport layer and preparation method | |
| CN107482124A (en) | A kind of method that steam auxiliary prepares perovskite solar cell | |
| CN110335945B (en) | Double-electron-transport-layer inorganic perovskite solar cell and manufacturing method and application thereof | |
| CN105355786A (en) | Method for preparing titanium dioxide and perovskite plane heterojunction solar cell at low temperature | |
| CN107768453A (en) | A kind of cadmium telluride thin-film battery with composite back electrode and preparation method thereof | |
| CN108649124B (en) | High-efficiency inorganic perovskite solar cell and preparation method thereof | |
| CN113193125A (en) | Flexible perovskite solar cell with high power-to-mass ratio and preparation method thereof | |
| CN106098948A (en) | The perovskite thin film of single step flash method growing large-size crystal grain and the preparation method of plane solaode | |
| CN101022136A (en) | Alkaline-earth metal salt decorative nano crystal semiconductor optical anode, producing method and application thereof | |
| CN101872685B (en) | Solid dye-sensitized nanocrystal/microcrystal silicon composite film solar cell and preparation method thereof | |
| CN107799654B (en) | High-efficiency planar perovskite solar cell and preparation method thereof | |
| CN111668340B (en) | Cd (cadmium) 3 Cl 2 O 2 Thin film, preparation method thereof and thin film solar cell | |
| CN105470338B (en) | A kind of flexible overlapping solar cell and preparation method | |
| CN110965074A (en) | Method for preparing composite film photoelectrode | |
| CN111326603A (en) | Preparation method of inorganic perovskite battery with zinc oxide as electron transport layer | |
| CN107705993B (en) | Dye-sensitized solar cells cupric oxide nano-rod array is to electrode and preparation method thereof | |
| CN103972398A (en) | Organic and inorganic hybridization solar cell and manufacturing method of organic and inorganic hybridization solar cell |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170704 |
|
| RJ01 | Rejection of invention patent application after publication |