CN110098333A - The processing method of the preparation method and perovskite solar battery of perovskite absorbed layer - Google Patents
The processing method of the preparation method and perovskite solar battery of perovskite absorbed layer Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of perovskite absorbed layer and the processing method of perovskite solar battery.The wherein preparation method of the perovskite absorbed layer includes the following steps: to form the process gas containing gaseous state organic source or the process gas containing inorganic source in gas generation cavity, and the temperature for controlling process gas reaches predetermined process temperature；Process gas is introduced into reaction chamber from gas generation cavity, so that the pressure in reaction chamber is reached default reaction pressure, temperature reaches default reaction temperature；It will be loaded in the substrate merging reaction chamber of inorganic thin film, react inorganic thin film with gaseous state organic source or inorganic source, so that perovskite absorbed layer be formed on the substrate.The preparation method of perovskite absorbed layer provided by the invention, gaseous state organic source or inorganic source are formed in independent airtight chamber and carry out gas-solid reaction, initial reaction stage is reduced because of the influence caused by gaseous state organic source or inorganic source density unevenness, improves the quality of perovskite absorbed layer.
Description
Technical field
The present invention relates to the preparation methods and perovskite of solar battery technology more particularly to a kind of perovskite absorbed layer too
The processing method of positive energy battery.
Background technique
Perovskite solar battery (perovskite solar cells) is the organic metal halogenation using Ca-Ti ore type
Solar battery of the object semiconductor as light absorbent.In recent years, the highest photoelectric conversion efficiency of perovskite solar battery from
3.8% has been increased to 23.2%.The photoelectric conversion efficiency has not exceeded only development other thin-film solar cells earlier, even more
It has forced the industrialization solar battery technology for being even more than the development many years such as polysilicon solar cell into a draw, has had huge
Industry development prospect.
Perovskite solar battery generally comprises two electrodes: transparent conducting glass and metal electrode are located at two electrodes
Between hole transmission layer and electron transfer layer (compacted zone) and hole transmission layer and electron transfer layer between perovskite inhale
Receive layer.Wherein the main function of perovskite absorbed layer is to absorb sunlight and generate electron-hole pair, and film quality is to calcium titanium
The photoelectric conversion efficiency of mine solar battery entirety influences very big.
The preparation of perovskite absorbed layer at this stage is mostly using liquid phase method or vapor phase method, wherein preparing using liquid phase method
During perovskite absorbed layer, various organic solvents are inevitably used, are had not to human health and Environmental security
Benefit influences, therefore liquid phase method is difficult to obtain large-scale application；And preparing perovskite absorbed layer using vapor phase method can avoid generating this
Class problem.It is mostly by gaseous organic source or inorganic source and to consolidate in the technology that existing vapor phase method prepares perovskite absorbed layer
The inorganic thin film of state carries out gas solid chemical reaction, obtains perovskite absorbed layer.It is described in patent application 201810257299.7
A kind of method that original position gas-solid reaction forms section perovskite absorbed layer, specifically puts organic source is opposite with the halide film of lead
It is placed in same airtight cavity, heating organic source is vaporized and reacts with the halide film of lead, forms final calcium
Titanium ore absorbed layer.There is vapor-phase reactant concentration not easy-regulating in this method, easily lead to deposition excessively, need to increase cleaning step
Suddenly, to increase process and cause the waste of raw material.Patent application 201610066196.3 is to prepare organic-inorganic perovskite thin
It is that lead oxide film is first prepared on electrically-conductive backing plate, then again through first after hydrogen halides (HCl, HBr or HI) steam steaming when film
Amine steam, ethamine steam or carbonamidine steam steaming prepare perovskite absorbed layer absorbed layer.This method step is relatively complicated, and
Equally exist vapor-phase reactant concentration not easy-regulating the problem of.Patent application 201580044633.5 is respectively by organic source power
AX and it is loaded with BX2The substrate of film is placed on the front-end and back-end of a chamber, passes through inert carrier gas in the environment of low pressure
Organic source power steam is loaded onto substrate surface and and BX2Film chemically reacts, and forms perovskite thin film.The preparation process
It equally exists perovskite caused by vapor-phase reactant is unevenly distributed in chamber and absorbs composition of layer unevenness, and then influence perovskite
The performance of solar battery.
Summary of the invention
In view of the foregoing drawbacks, the present invention provides a kind of preparation method of perovskite absorbed layer, independent and two connection
It is respectively formed the process gas containing vapor-phase reactant in airtight chamber and carries out reacting for vapor-phase reactant and inorganic thin film, reduces
Initial reaction stage improves the quality of perovskite absorbed layer because of the influence caused by vapor-phase reactant density unevenness.
The present invention provides a kind of system for realizing above-mentioned preparation method.
The present invention also provides a kind of processing methods of perovskite solar battery, including prepare calcium according to aforementioned preparation process
Titanium ore absorbed layer, so as to obtain perovskite solar battery of good performance.
To achieve the above object, the first aspect of the invention is to provide a kind of preparation method of perovskite absorbed layer, packet
Include following steps:
The process gas of the organic source containing gaseous state or the process gas containing inorganic source are formed in gas generation cavity, and control work
The temperature of skill gas reaches predetermined process temperature；
The process gas for being up to predetermined process temperature introduces reaction chamber from gas generation cavity, and reaches the pressure in reaction chamber
Reach default reaction temperature to default reaction pressure, temperature；
It will be loaded in the substrate merging reaction chamber of inorganic thin film, make inorganic thin film and gaseous state organic source or inorganic source default
It is reacted under reaction temperature and default reaction pressure, so that perovskite absorbed layer be formed on the substrate.
Technical solution provided by the invention forms the process gas of gaseous state organic source in gas generation cavity or contains inorganic source
Process gas after the temperature and pressure in reaction chamber all reaches default reaction condition, then will be loaded with subsequently into reaction chamber
In the substrate merging reaction chamber of inorganic thin film, occur that gaseous state organic source or inorganic source under default reaction condition with inorganic thin film
Reaction, avoid prepared in single airtight chamber at this stage perovskite absorb layer process in initial reaction stage because vapor-phase reactant is close
Perovskite absorbs the problem of composition of layer unevenness caused by being unevenly distributed in closed chamber.
And during entire gas-solid reaction carries out, can control gaseous state by conditions such as temperature in gas generation cavity has
The generating rate of machine source or inorganic source, it is ensured that gas-solid reaction obtains more accurately controlling, and carries out gas-solid reaction more steady
It is fixed, smooth, finally make the entire perovskite absorbed layer obtained that there is highly uniform structure, can especially improve is that perovskite is inhaled
The uniformity that layer is longitudinally formed process is received, so that perovskite absorbed layer is preferably played photoelectric converting function, and then improve calcium
The photoelectric conversion efficiency of titanium ore solar battery.
In the present invention, above-mentioned organic source and inorganic source and solid film be may each be in current perovskite solar battery
Raw material used in perovskite absorbed layer.It is broadly divided into following three kinds of situations:
1) organic source is aminated compounds and/or amidine compound, and inorganic thin film has CBX3Composition.Common amine
Compound such as can be methylamine, ethamine, and common amidine compound such as can be carbonamidine；In the composition of inorganic thin film, B generation
The one or more divalent metals of table, such as lead, tin, copper, zinc, palladium, cadmium, mercury；C represents the monovalence of monovalent metal and hydrogen atoms
One of cation is a variety of, such as hydrogen ion (H+), ammonium ion (NH4 +) etc.；X represents halide ion (such as I-、Br-), sulphur
One of cyanogen root, cyanogen root and oxygen cyanogen root are a variety of.
For example organic source is CH3NH2, the group of inorganic thin film is as HPbI3, the two generation gas-solid reaction generation
CH3NH3PbI3。
2) organic source has the composition of AX, and inorganic thin film has BX2Composition, the two reaction generate ABX3, wherein A is represented
Amino (amido) or amidino groups；B represents one or more divalent metals, and X is represented in halide ion, thiocyanate, cyanogen root and oxygen cyanogen root
It is one or more.
For example organic source is CH3NH3The group of I, inorganic thin film become PbI2, the two reaction generation CH3NH3PbI3。
3) inorganic source is the composition with DX, and D represents one or more alkali metal, such as caesium, rubidium, potassium；Inorganic thin film tool
There is BX2Composition, wherein representing one or more divalent metals, X is represented in halide ion, thiocyanate, cyanogen root and oxygen cyanogen root
It is one or more.
In addition to the foregoing, inorganic thin film can also be DX and BX2Laminated film, such as cesium iodide CsI and iodate
Lead PbI2Laminated film.
It is appreciated that in actual production, if desired there are two types of or more kinds of gaseous state organic sources participate in reaction, Huo Zhexu
There are gaseous state organic source and inorganic source to participate in reaction, the gas generation cavity of multiple parallel connections, each gas generation cavity also can be set
Process gas needed for interior each self-forming, is then introduced into reaction chamber and reacts with inorganic thin film.
In specific implementation process of the present invention, the process gas containing gaseous state organic source is formed in gas generation cavity or is contained
There is the process gas of inorganic source, can be determined according to organic source and the property of inorganic source, can specifically include following several situations:
Situation 1: the gas generation cavity will be injected in gaseous organic source；I.e. organic source is gaseous state at normal temperature, can be adopted
With modes such as pressure pan decompression releases, organic source is injected into gas generation cavity.It is released stress and the factors such as flow, control by control
The synthesis speed of gaseous state organic source processed.
Situation 2: it will be placed in gas generation cavity in the organic source of solid-state or liquid, it is organic that heating forms it into gaseous state
Source；If organic source is solid-state or liquid at normal temperature, the mode of heat temperature raising can be used, it is made to become gaseous state.Pass through control
Temperature in gas generation cavity, can control solid-state or liquid organic source is converted into the rate of gaseous state organic source.
Situation 3: the solution dissolved with organic source is placed in gas generation cavity, and heating up makes organic source be precipitated and form gas
State organic source.By the temperature in control gas generation cavity, the precipitation rate of organic source can be controlled.
Situation 4: the solution dissolved with inorganic source is placed in gas generation cavity, passes through carrier gas molten dissolved with inorganic source
Liquid forms the air-flow for having inorganic source.Specifically, carrier gas can be made by the aforementioned solution dissolved with inorganic source, take carrier gas
Air-flow with inorganic source and solute, as containing the process gas of inorganic source.By control carrier gas flow and carrier gas with
The liquid level area of above-mentioned solution contact, can control the generating rate of inorganic source.
In situation 4, if the flow of carrier gas is very big, process gas is formed by gas generation cavity and is actually similar to
Spraying, process gas at this time is made of the droplet of the inorganic source and solute that carry in carrier gas and carrier gas.For convenience of saying
Bright, inorganic source is still known as " gas-solid reaction " with reacting for solid film by the present invention.
In specific implementation process of the present invention, for afore-mentioned 1 to situation 3, the organic source in process gas is in gaseous state,
During gas-solid reaction, usually controls the temperature in gas generation cavity and reach predetermined process temperature, the partial pressure of process gas stablizes dimension
It holds in saturated vapour pressure, it is ensured that process gas, especially organic source enter reaction chamber with constant rate.
It is appreciated that can control the synthesis speed of gaseous state organic source, to be conducive to control by control heating temperature
Subsequent gas-solid reaction process.Especially, when organic source is liquid or solid-state at normal temperature, then in gas generation cavity process gas temperature
Degree can be controlled in predetermined process temperature, and partial pressure then can be controlled in saturated vapour pressure.
In some embodiments of the invention, above-mentioned process gas can be only gaseous state organic source；In other implementations of the present invention
It is that carrier gas is passed through into gas generation cavity in example, carrier gas and gaseous state organic source or carrier gas and inorganic source (and solute) are common
Constitute process gas.In addition, by controlling the flow of carrier gas, being not only contributed to accurate by being passed through carrier gas into gas generation cavity
The composition of process gas is controlled, and is conducive to control the speed that process gas, especially gaseous state organic source or inorganic source enter reaction chamber
Rate, to more accurately control the rate of gas-solid reaction.
Specifically, the flow of controllable carrier gas is 0~10000sccm.In specific implementation process of the present invention, for experiment
The small scale experiments of room rank can be without using carrier gas (i.e. the flow of carrier gas is 0) or control if the reactant selected is organic source
The flow of carrier gas processed is smaller.For large-scale industrial production, either gaseous state organic source or inorganic source, it is both needed to be passed through load
Gas, flow general control is in 10~10000sccm.
Above-mentioned carrier gas can be carrier gas commonly used in the art, such as nitrogen and helium, neon, in the inert gases such as argon gas
It is one or more.
It is appreciated that be the temperature fluctuation that process gas is caused after avoiding carrier gas from entering gas generation cavity, it can be in advance to carrier gas
It is heated, the temperature of carrier gas is made to reach predetermined process temperature.Such as it can be on the pipeline between carrier gas source and gas generation cavity
Heating device is set, increases temperature in carrier gas transport process, reaches predetermined process temperature.
When the process gas in gas generation cavity reaches predetermined process temperature and stabilization, process gas can be introduced reaction chamber,
The pressure in reaction chamber is set to reach default reaction pressure, temperature reaches default reaction temperature.It has been observed that the temperature in gas generation cavity
Degree is determined according to organic source or the property of inorganic source.In specific implementation process of the present invention, gas generation cavity is usually controlled
Interior temperature is 50~300 DEG C.
And the temperature and pressure in reaction chamber is then determined according to practical gas-solid reaction condition, wherein default reaction temperature is specific
It can be 50~300 DEG C.In specific implementation process of the present invention, the temperature in usual gas generation cavity is different from reaction chamber
Temperature, i.e. predetermined process temperature are different from default reaction temperature.In order to avoid the process gas from gas generation cavity is entering instead
Temperature fluctuation is caused when answering chamber, gas-heating apparatus generally need to be also equipped between gas generation cavity and reaction chamber, such as in gas
It is enclosed on pipeline between body generation cavity and reaction chamber and sets heating coil, process gas is made to reach default in transport process in pipeline
Reaction temperature.
Default reaction pressure can be high pressure or low pressure, i.e. gas-solid reaction can react under high pressure or under vacuum environment,
The pressure of its mesohigh is 0.1013MPa~1MPa, i.e. a normal atmosphere is depressed into 1MPa；The pressure of low pressure is generally not less than
0.1Pa and less than one standard atmospheric pressure.
When the temperature and pressure in reaction chamber respectively reaches above-mentioned default reaction temperature and default reaction pressure condition, then
It can will be loaded in the substrate merging reaction chamber of inorganic thin film, gas-solid reaction occur, wherein the time of gas-solid reaction can be according to reality
The factors such as the composition of the thickness of requirement, inorganic thin film, the composition of inorganic thin film, gaseous state organic source for perovskite absorbed layer are closed
Reason setting, usually can be 1~120min.
During gas-solid reaction, in order to maintain default reaction temperature constant, temperature control equipment can be set in reaction chamber.
If gas-solid reaction is to complete under low pressure, need through the continuous vacuumize process of vacuum plant, it is ensured that the pressure dimension in reaction chamber
It is fixed to keep steady；And if gas-solid reaction is to complete under high pressure, to avoid hypertonia, can also appropriate pressure release, to ensure reaction chamber
Interior pressure maintains to stablize.
In addition, part flow arrangement can also be arranged in reaction chamber, the process gas from gas generation cavity is enable to be uniformly distributed
In reaction chamber.
Further, after the pressure in reaction chamber reaches default reaction pressure, temperature reaches default reaction temperature, also
Process gas can be stablized into 0.1~60min in reaction chamber first, it is then again that the substrate merging for being loaded with inorganic thin film is described anti-
It answers intracavitary.
So-called " stabilization " is actual industrial term, exactly makes the process gas in reaction chamber in default reaction pressure and presets
A period of time is maintained under reaction temperature, it is ensured that the process gas in reaction chamber is uniformly distributed in entire reaction chamber, and ingredient is more equal
It is even, it is more uniform to further ensure that gas-solid reaction initial stage is formed by perovskite absorbed layer.
Optionally, after the reaction was completed, it can also be made annealing treatment according to actual needs, usually according to annealing front and back
The performance test results of perovskite solar battery determine the need for implementing annealing.Annealing temperature is specifically as follows 50~
300 DEG C, and annealing temperature is lower than default reaction temperature.
The second aspect of the invention is to provide a kind of system for realizing preparation method described in first aspect, including vacuum
Device, series connection and the first airtight cavity and the second airtight cavity be connected, along the trend of process gas, the first airtight cavity is gas
Generation cavity, the second airtight cavity are reaction chamber, and wherein gas generation cavity is equipped with temperature control equipment, and reaction chamber is controlled equipped with temperature
Device, pressure control device and gas diverter, vacuum plant are connected to the first airtight cavity or the second airtight cavity.
The third aspect of the invention is to provide a kind of processing method of perovskite solar battery, includes the following steps:
One of electron transfer layer and hole transmission layer and inorganic thin film are sequentially formed on substrate；
According to preparation method described in first aspect, perovskite absorbed layer is formed on the substrate；
Another in electron transfer layer and hole transmission layer and electrode is finally sequentially formed on perovskite absorbed layer.
Specifically, substrate used in processing perovskite solar battery, can be institute in current perovskite solar battery
Common transparent conductive substrate, such as transparent FTO glass, transparent AZO glass, transparent ito glass, PET flexible transparent conducting film
Or PI flexible transparent conducting film.
Electron transfer layer, hole transmission layer, inorganic thin film, electrode can be prepared using this field conventional means, such as
Can be by processes such as spin-coating method, cladding process, vacuum methodes, wherein the thickness of inorganic thin film specifically can be 0.05~1 μm.
Organic source/inorganic source and inorganic thin film are placed in solely by the preparation method of perovskite absorbed layer provided by the invention
In vertical airtight cavity, complete the formation of gaseous state organic source/inorganic source and gas-solid reaction in different airtight cavities respectively,
In this way before gas-solid reaction, the state of the process gas in reaction chamber reaches stable default reaction temperature and default reaction pressure
Power solves perovskite absorbed layer caused by vapor-phase reactant uneven concentration when heating under same airtight cavity and is distributed not
Equal problem；Also, pass through control gaseous state organic source/synthesis speed of inorganic source, reaction time, reaction pressure, reaction temperature
Deng being accurately controlled gas-solid reaction process, it is ensured that gas-solid reaction is carried out with steady rate, so that entire perovskite absorbed layer be made to have
There is more uniform ingredient, perovskite absorbed layer is made preferably to play photoelectric converting function, improves perovskite solar battery
Performance.
Provided by the present invention for implementing the system of above-mentioned preparation method, structure is simple, can absorb in existing perovskite
It is improved on the basis of layer preparation system.
The processing method of perovskite solar battery provided by the invention, the preparation side including above-mentioned perovskite absorbed layer
Method, so that making the property of perovskite solar battery can be promoted.
Detailed description of the invention
Fig. 1 is the system structure diagram for being used to prepare perovskite absorbed layer provided in a specific embodiment of the invention；
Fig. 2 is the system structure signal for being used to prepare perovskite absorbed layer provided in another specific embodiment of the present invention
Figure.
Description of symbols:
10- vacuum plant；20- gas generation cavity；21- air inlet pipeline；
22- gas flowmeter；23- valve；24- heating coil；
25- gas stirring device；26- air delivering pipeline；30- reaction chamber；
31- gas diverter；32- gas exhaust piping；33- relief valve；
34- air inlet pipeline；35- valve；40- carrier gas source；
50- exhaust gas processing device；61- preloads chamber；62- unloads chamber；
63- air inlet pipeline；64- gas exhaust piping；65- valve.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment one
Fig. 1 and Fig. 2 is respectively the system knot that perovskite absorbed layer is used to prepare provided in the specific embodiment of the invention
Structure schematic diagram.As depicted in figs. 1 and 2, the present embodiment provides a kind of systems for being used to prepare perovskite absorbed layer, including vacuum holding
The first airtight cavity and the second airtight cavity for setting 10, series connection and conducting, along the trend of process gas, the first airtight cavity is gas
Generation cavity 20, the second airtight cavity are reaction chamber 30, and wherein gas generation cavity 20 is equipped with temperature control equipment (not shown), reaction
Chamber 30 is equipped with temperature control equipment (not shown), pressure control device (not shown) and gas diverter 31, vacuum plant 10
It is connected to the first airtight cavity and/or the second airtight cavity.
Specifically, above-mentioned the first airtight cavity and the second closed chamber respectively as gas generation cavity 20 and reaction chamber 30
Body may each be currently used for airtight cavity commonly used by processing perovskite absorbed layer, specifically can be flat cavity, can also
To be tubular type cavity.The size of airtight cavity can be suitble to industrialization area battery to produce, and can also be suitble to laboratory small area
Battery scientific research.
As shown in Figure 1, the quantity of above-mentioned gas generation cavity 20 can be one；Or as shown in Fig. 2, above-mentioned gas occurs
The quantity of chamber 20 is also possible to two or more, and it is reasonable to be specifically arranged according to the factors such as gaseous state organic source or the type of inorganic source
The quantity of gas generation cavity 20.Wherein, when the quantity of gas generation cavity 20 is multiple, multiple 20 parallel connections of gas generation cavity are set
It sets, and each gas generation cavity 20 is connected to reaction chamber 30 respectively.
Temperature control equipment is used to control the temperature in gas generation cavity 20 and reaction chamber 30.The present embodiment is for above-mentioned temperature
Degree control device is not specially limited, and can be the heating equipment with above-mentioned first airtight cavity and the cooperation of the second airtight cavity.
Please further refer to Fig. 1 and Fig. 2, above system can also include carrier gas source 40, specifically, gas generation cavity 20 can
It is connected to by air inlet pipeline 21 with carrier gas source 40, the carrier gas in carrier gas source 40 is enable to enter gas via air inlet pipeline 21
Chamber 20.
Further, gas flowmeter 22 and valve 23 can be also equipped on above-mentioned air inlet pipeline 21, wherein gas flowmeter
22 are used to control the flow of carrier gas for the flow to measure carrier gas, valve 23.
Further, can also be twined on above-mentioned air inlet pipeline 21 equipped with heating coil 24, with to flowing in air inlet pipeline 21
Carrier gas heated, make carrier gas enter gas generation cavity 20 before reach predetermined process temperature.
Further, gas stirring device 25 can be also equipped in above-mentioned gas generation cavity 20, in gas generation cavity
Process gas is stirred, and mixes carrier gas quickly with gas organic source or inorganic source, and makes process gas in entire gas generation cavity
It is quickly evenly distributed in 20.
It is connected to specifically, can be realized by air delivering pipeline 26 between above-mentioned gas generation cavity 20 and reaction chamber 30.Further
, it also is provided with valve 23 on the air delivering pipeline 26 and twines equipped with heating coil 24, wherein valve 23 is for adjusting air delivering pipeline 26
The flow of interior process gas, heating coil 24 are used to heat process gas of the flowing in air delivering pipeline 26, reach its temperature
To default reaction temperature.
Gas diverter 31 can be equipped in above-mentioned reaction chamber 30, process gas in this way from gas generation cavity 20 can be
It is evenly distributed under the action of part flow arrangement 31 in reaction chamber 30.
As previously mentioned, reaction chamber 30 is equipped with pressure control device.The present embodiment is not spy for above-mentioned pressure control device
It does not limit, can be the pressure control equipment with airtight cavity cooperation.Please further refer to Fig. 1 and Fig. 2, reaction chamber 30 is connected with
Gas exhaust piping 32 is equipped with relief valve 33 on the gas exhaust piping 32, when the pressure in reaction chamber 30 is more than default reaction pressure, opens
Relief valve 33 is opened, the gas in reaction chamber 30 is discharged by gas exhaust piping 32.
I.e. relief valve 33 is used as pressure control device.In the specific implementation process, relief valve 33 is usually in high-pressure situations
Lower use, i.e., default reaction pressure is more than 1 standard atmospheric pressure.
Above-mentioned relief valve 32 especially can be automatic pressure relief valve, be more than default reaction pressure with the pressure in reaction chamber 30
When, automatic pressure relief valve automatically turns on and discharge part gas, it is ensured that the pressure in reaction chamber 30 is stably maintained at default reaction pressure
Power.
When gas-solid reaction is to carry out under vacuum conditions, i.e., default less than 1 atmospheric pressure of reaction pressure, then in entire gas-solid
During reaction carries out, vacuum plant 10 can be kept to open.Therefore, vacuum plant 10 can be passed through gas exhaust piping 32 and reaction chamber
30 connections.
Specifically, the vacuum plant 10 can be this fields such as vacuum pump conventional vacuum equipment, as long as can ensure gas-solid
Air, the moisture etc. in system are discharged before reaction, and ensure that the gas-solid reaction carried out under vacuum condition can be gone on smoothly
?.
With further reference to Fig. 1 and Fig. 2, which may also include exhaust gas processing device 50, which specifically may be used
To be connected to by gas exhaust piping 32 with reaction chamber 30.In this way, the gas being discharged in autoreaction chamber 30 can be in exhaust gas processing device
It is recycled and is handled in 50, especially after the reaction in reaction chamber 30 is completed, reaction end gas can be via gas exhaust piping
It is handled and is recycled in 32 entrance exhaust gas processing devices 50.
Please further refer to Fig. 1 and Fig. 2, which specifically be can connect in reaction chamber 30 and vacuum plant
Between 10, so before reactions, air, the vapor etc. in exhaust gas processing device 50 can be discharged together.
Since the gas as carrier gas is generally nitrogen or inert gas, reaction chamber 30 can pass through air inlet pipeline 34
It is connected to carrier gas source 40, nitrogen or inert gas in carrier gas source 40 is enable to enter reaction chamber 30 via air inlet pipeline 34.This
Sample can be passed through inert gas or nitrogen into reaction chamber 30 by air inlet pipeline 34 before gas-solid reaction；It is carried out in gas-solid reaction
In the process, can also by air inlet pipeline 34 into reaction chamber 30 topping up or nitrogen.
Further, valve 35 can also be equipped on air inlet pipeline 34, to adjust the flow of nitrogen or inert gas.
Please further refer to Fig. 1 and Fig. 2, above system can also include the preloading chamber 61 connecting with reaction chamber 30 and unloading
Chamber 62.Before gas-solid reaction, the substrate for being loaded with inorganic thin film well prepared in advance can be placed in preloading chamber 61 first, and right
It preloads chamber 61 to carry out vacuumizing heating, respectively reaches default reaction temperature and default reaction to the temperature and pressure in reaction chamber 30
After pressure, inorganic thin film will be loaded with and be sent into reaction chamber 30 by preloading chamber 61, inorganic thin film and gaseous state organic source or inorganic are made
Source carries out gas-solid reaction；After completing to gas-solid reaction, the substrate for being formed with perovskite absorbed layer is entered by reaction chamber 30 to be unloaded
Chamber 62, operator or automatic production line can take out the substrate for being formed with perovskite absorbed layer in self-unloading chamber 62.
Further, above-mentioned preloading chamber 61 and unloading chamber 62 can pass through corresponding air inlet pipeline 63 and carrier gas source 40 respectively
Connection, preloading chamber 61 and unloading chamber 62 can be connect by corresponding gas exhaust piping 64 with vacuum plant 10 respectively.In air inlet pipe
Road 63 and gas exhaust piping 64 can be equipped with valve 65.
Embodiment two
The present embodiment provides a kind of preparation methods of perovskite absorbed layer, are the reactions completed under high pressure approach, for side
Just understand, be illustrated, specifically comprise the following steps: below with reference to the system in previous embodiment one
1, conductive substrates well prepared in advance, being loaded with hole transmission layer (or electron transfer layer) and inorganic thin film are set
In preloading chamber 61；Liquid or solid-state organic source are placed in gas generation cavity 20, or will at room temperature be in gaseous organic source
It accesses in gas generation cavity 20.
2, vacuum plant 10 is opened, whole system is vacuumized, turns off vacuum plant 10, opens carrier gas source 40 with to being
Carrier gas is filled in system.Repetition is vacuumized and is filled with carrier gas 1~10 time, by system oxygen and vapor etc. may influence reaction
The gas of process is sufficiently discharged.
Specifically, can vacuumize first makes the pressure in gas generation cavity 20 and reaction chamber 30 reach 10-2~1torr, then
It is passed through carrier gas, the pressure in gas generation cavity 20 and reaction chamber 30 is made to reach 760torr (i.e. a standard atmospheric pressure).
3, heat gas generation cavity 20 makes liquid or the solid-state organic source in gas generation cavity 20 be converted into gaseous state, gas
Temperature in generation cavity 20 reaches predetermined process temperature, such as 50~300 DEG C, and process gas divides the saturated vapor for reaching organic source
Pressure.
4, reaction chamber 30 is heated, and under the action of carrier gas, makes the gaseous state organic source in gas generation cavity 20 in carrier gas
Enter reaction chamber 30 through air delivering pipeline 26 under carrying, carrier gas flux can be 10~10000sccm, uniformly divide through part flow arrangement 31
Cloth makes to reach default reaction temperature (such as 50~300 DEG C) and default reaction pressure ratio in reaction chamber 30 in reaction chamber 30
For example a normal atmosphere is depressed into 1Mpa.
After stablizing about 0.1~60min, the substrate in preloading chamber 61 is sent into reaction chamber 30, preparatory shape on the substrate
At having electron transfer layer (or hole transmission layer) and inorganic thin film, react inorganic thin film with gaseous state organic source, the reaction time
For 1~120min, reaction temperature is above-mentioned default reaction temperature, and reaction pressure is above-mentioned default reaction pressure to form calcium titanium
Mine absorbed layer.
While reacting progress, continue to be passed through carrier gas into reaction chamber 30 by air inlet pipeline 34.If in reaction chamber 30
Pressure be more than default reaction pressure, then open relief valve 33, the gas in reaction chamber 30 made to enter tail gas through gas exhaust piping 32
Processing unit 50.
5, the temperature after the reaction was completed, adjusted in reaction chamber 30 is made annealing treatment, and annealing temperature is 50~300 DEG C of (roots
According to actual conditions, step 5 can be omitted).
6, after the completion of making annealing treatment, the tail gas in reaction chamber 30 is extracted out, enters exhaust gas processing device through gas exhaust piping 32
50.In exhaust gas processing device 60, can by cooling, make wherein unreacted gaseous state organic source become liquid or solid-state, and carry
Gas can then be discharged into atmosphere or be discharged into atmosphere after processing.
The substrate for being formed with perovskite absorbed layer enters unloading chamber 62, takes out.
Embodiment three
The present embodiment provides a kind of preparation methods of perovskite absorbed layer, are the reactions completed under vacuum conditions, for side
Just understand, be illustrated, specifically comprise the following steps: below with reference to the system in previous embodiment one
1, conductive substrates well prepared in advance, being loaded with hole transmission layer (or electron transfer layer) and inorganic thin film are set
In preloading chamber 61；Liquid or solid-state organic source are placed in gas generation cavity 20 or gaseous state organic source accesses gas
In chamber 20.
2, vacuum plant 10 (such as vacuum pump) is opened, whole system is vacuumized, turn off vacuum plant 10, opened and carry
Gas source 40 is to be filled with carrier gas into system.Repetition is vacuumized and is filled with carrier gas 1~10 time, by the oxygen and vapor etc. in system
The gas that may influence reaction process is sufficiently discharged.
Carrier gas source 30 is closed, vacuum pump is opened, make less than one standard atmospheric pressure of the pressure of total system, for example be greater than etc.
In 0.1Pa and less than one standard atmospheric pressure.
3, the valve 23 on valve 23 and air delivering pipeline 26 on air inlet pipeline 21 is closed, to ensure gas generation cavity 20
It is interior to be in vacuum state, and the process gas in subsequent gases generation cavity 20 is avoided to enter reaction chamber under the action of vacuum plant 10
30.Heat gas generation cavity 20 makes to be in a liquid state in gas generation cavity 20 or solid organic source rapidly goes to gaseous state, and gas occurs
Temperature in chamber 20 reaches predetermined process temperature, such as 50~300 DEG C, and process gas divides the saturated vapour pressure for reaching organic source.
4, reaction chamber 30 is heated, and is opened on the valve 23 on air inlet pipeline 21 and heating coil 24 and air delivering pipeline 26
Valve 23 and heating coil 24, so that carrier gas in carrier gas source 40 is entered gas generation cavity 20 through air inlet pipeline 21, and carry
Gaseous state organic source enters reaction chamber 30 through air delivering pipeline 26, then is evenly distributed in reaction chamber 31 through part flow arrangement 31, makes to react
Reach default reaction temperature (such as 50~300 DEG C) and default reaction pressure in chamber 30, such as more than or equal to 0.1Pa and less than one
A standard atmospheric pressure.
After stablizing about 0.1~60min, the substrate in preloading chamber 61 is sent into reaction chamber 30, is made inorganic on substrate
Film is reacted with gaseous state organic source, and the reaction time is 1~120min, to form perovskite absorbed layer.
While reacting progress, vacuum plant 10 is continued working with the pressure in maintenance system, especially reaction chamber 30
Interior pressure is more than or equal to 0.1Pa and less than one standard atmospheric pressure.
5, the temperature after the reaction was completed, adjusted in reaction chamber 30 is made annealing treatment, and annealing temperature is 50~300 DEG C of (roots
According to actual conditions, step 5 can be omitted).
6, after the completion of making annealing treatment, the tail gas in reaction chamber 30 is extracted out, enters exhaust gas processing device through gas exhaust piping 32
50, for example, can by cooling, lower than the freezing point of gaseous state organic source, make wherein unreacted gaseous state organic source become liquid or solid
State, and carrier gas can be then discharged into atmosphere.
The substrate for being formed with perovskite absorbed layer enters unloading chamber 62, takes out.
Example IV
The present embodiment provides a kind of processing methods of perovskite solar battery, include the following steps:
Electron transfer layer (or hole transmission layer) and inorganic thin film are sequentially formed on substrate；
According to the preparation method that previous embodiment two or embodiment three provide, perovskite absorbed layer is formed；
Hole transmission layer (or electron transfer layer) is formed on perovskite absorbed layer, re-forms metal electrode.
Below by way of concrete case, elaborate to the processing method of perovskite solar battery:
Case 1
Using transparent ito glass as substrate, electron transfer layer is first prepared on ito glass, then prepare PbI2Film (i.e. BX2It is thin
Film).
With CH3NH3I is organic source (i.e. AX), and the step 1 provided according to previous embodiment two is to step 6, in electron-transport
Perovskite absorbed layer CH is formed on layer3NH3PbI3。
In CH3NH3PbI3It is sequentially prepared hole transmission layer and electrode on film, obtains perovskite solar battery.
Case 2
Using transparent ito glass as substrate, first prepare to form electron transfer layer on ito glass, then prepare PbI2Film is (i.e.
BX2Film).
According to the preparation method provided in embodiment two, perovskite absorbed layer is formed on the electron transport layer, wherein with
CH3NH3I and CH (NH2)2Two kinds of solid organic matters of I are organic source (i.e. AX), and perovskite absorbed layer (CH is prepared3NH3)x CH
(NH2)1-xPbI3Film, wherein 0 < x < 1.
Hole transmission layer and metal electrode are formed on perovskite absorbed layer, obtain perovskite solar battery.
Case 3:
Using transparent ito glass as substrate, electron transfer layer is first prepared on ito glass, then prepare PbI2It is compound with CsBr
Film.
With CH3NH3I and CH (NH2)2I is organic source, and the step 1 provided according to previous embodiment two is to step 6, in electronics
Perovskite absorbed layer Cs is formed in transport layerx(CH3NH3)y(CH(NH2)2)1-x-yPb(IzBr1-z)3, wherein 0 < x <, 1,0 < y <
1,0 < z < 1, x+y < 1.
Hole transmission layer and metal electrode are formed on perovskite absorbed layer, obtain perovskite solar battery.
Case 4:
Using transparent ito glass as substrate, electron transfer layer and PbI are sequentially formed on ito glass2Film (i.e. BX2It is thin
Film).
With CH3NH3I is organic source (i.e. AX), according to the step 1 in previous embodiment three to step 6, in electron transfer layer
Upper formation perovskite absorbed layer CH3NH3PbI3。
Hole transmission layer and electrode are sequentially formed on perovskite absorbed layer, obtains perovskite solar battery.
Case 5:
Using transparent ito glass as substrate, hole transmission layer and PbI are sequentially formed on ito glass2Film (i.e. BX2It is thin
Film).
With CH3NH3I and CH (NH2)2Two kinds of substances of I are organic source (i.e. AX), according to the step 1 in embodiment three to step
6, perovskite absorbed layer (CH is made3NH3)x(CH(NH2)2)1-xPbI3, wherein 0 < x < 1.
Electron transfer layer and metal electrode are sequentially formed on perovskite absorbed layer, obtains perovskite solar battery.
Case 6:
Using transparent ito glass as substrate, electron transfer layer and PbI are sequentially formed on ito glass2It is compound with CsBr
Film.
According to the step 1 in embodiment three to step 6, with CH3NH3I and CH (NH2)2Organic source is used as in two kinds of substances of I,
Perovskite absorbed layer Cs is madex(CH3NH3)y(CH(NH2)2)1-x-yPb(IzBr1-z)3, wherein 0 < x <, 1,0 < y <, 1,0 < z <
1, x+y < 1.
Hole transmission layer and conductive electrode are sequentially formed on perovskite absorbed layer, obtains perovskite solar battery.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of preparation method of perovskite absorbed layer, which comprises the steps of:
The process gas containing gaseous state organic source or the process gas containing inorganic source are formed in gas generation cavity, and described in control
The temperature of process gas reaches predetermined process temperature；
The process gas for being up to predetermined process temperature introduces reaction chamber from gas generation cavity, makes the pressure in the reaction chamber
Reach default reaction pressure, temperature reaches default reaction temperature；
The substrate that inorganic thin film will be loaded with is placed in the reaction chamber, makes inorganic thin film and the gaseous state organic source or described inorganic
Source is reacted under the default reaction temperature and default reaction pressure, to form perovskite absorbed layer over the substrate.
2. preparation method according to claim 1, which is characterized in that the organic source is aminated compounds and/or amidine class
Compound, the inorganic thin film have CBX3Composition, wherein B represents one or more divalent metals, and C represents hydrogen atoms
One of monovalent cation is a variety of, and X represents one of halide ion, thiocyanate, cyanogen root and oxygen cyanogen root or a variety of；
Alternatively, the organic source has the composition of AX, wherein A represents amino or amidino groups, and the inorganic thin film has BX2Composition；
The inorganic source is the composition with DX, and wherein D represents one or more alkali metal, and the inorganic thin film has BX2Group
At.
3. preparation method according to claim 1 or 2, which is characterized in that described formed in gas generation cavity contains gas
The process gas of state organic source or process gas containing inorganic source, comprising:
The gas generation cavity will be injected in the gaseous organic source；Alternatively,
It will be placed in the gas generation cavity in the organic source of solid-state or liquid, heating forms it into gaseous state organic source；Or
Person,
Solution dissolved with the organic source is placed in the gas generation cavity, and heating up makes the organic source be precipitated and be formed
Gaseous state organic source；Alternatively,
Solution dissolved with the inorganic source is placed in the gas generation cavity, makes carrier gas by being dissolved with the inorganic source
Solution forms the air-flow for having the inorganic source.
4. preparation method according to claim 1 or 3, which is characterized in that described formed in gas generation cavity contains gas
The process gas of state organic source or process gas containing inorganic source, further includes: with the flow of 0~10000sccm to the gas
Carrier gas is passed through in generation cavity；
The carrier gas and the gaseous state organic source collectively form the process gas or the process gas includes the carrier gas and institute
State inorganic source.
5. preparation method according to claim 1-4, which is characterized in that the predetermined process temperature be 50~
300℃。
6. preparation method according to claim 1, which is characterized in that the default reaction temperature is 50~300 DEG C, described
Reaction time is 1~120min, and the default reaction pressure is high pressure or low pressure, the pressure of mesohigh is 0.1013~
The pressure of 1MPa, the low pressure are not less than 0.1Pa and less than 1 standard atmospheric pressure.
7. preparation method according to claim 1, which is characterized in that the pressure in reaction chamber reaches default reaction pressure
Power, temperature reach after default reaction temperature, further includes: the process gas are stablized 0.1~60min in reaction chamber, then
The substrate for being loaded with inorganic thin film is placed in the reaction chamber again.
8. preparation method according to claim 1-7, which is characterized in that after reaction completion, also wrap
The step of including annealing, annealing temperature is 50~300 DEG C, and the annealing temperature is lower than the default reaction temperature.
9. a kind of system for realizing any one of claim 1-8 preparation method, which is characterized in that including vacuum plant, string
Connection and the first airtight cavity and the second airtight cavity of conducting, along the trend of the process gas, first airtight cavity is institute
Gas generation cavity is stated, second airtight cavity is the reaction chamber, wherein the gas generation cavity is equipped with temperature control equipment,
The reaction chamber is equipped with temperature control equipment, pressure control device and gas diverter, the vacuum plant and first closed
Cavity or the connection of the second airtight cavity.
10. a kind of processing method of perovskite solar battery, which comprises the steps of:
One of electron transfer layer and hole transmission layer and inorganic thin film are sequentially formed on substrate；
According to the described in any item preparation methods of claim 1-8, perovskite absorbed layer is formed over the substrate；
Finally another in electron transfer layer and hole transmission layer and electrode is sequentially formed on the perovskite absorbed layer.
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| CN113471367A (en) * | 2021-06-30 | 2021-10-01 | 无锡极电光能科技有限公司 | System and method for preparing perovskite film layer and application thereof |
| CN113644209A (en) * | 2021-08-11 | 2021-11-12 | 无锡极电光能科技有限公司 | Preparation method and preparation device of perovskite film layer and perovskite solar cell |
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