CN107887514A - A kind of preparation method and applications of perovskite thin film - Google Patents
A kind of preparation method and applications of perovskite thin film Download PDFInfo
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- CN107887514A CN107887514A CN201711104063.1A CN201711104063A CN107887514A CN 107887514 A CN107887514 A CN 107887514A CN 201711104063 A CN201711104063 A CN 201711104063A CN 107887514 A CN107887514 A CN 107887514A
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- 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
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
The present invention relates to a kind of preparation method and applications of perovskite thin film.The preparation method of perovskite thin film comprises the steps of：(1) perovskite precursor solution is prepared；(2) in the case where substrate heats, the brush for being impregnated with perovskite precursor solution is brushed into substrate surface with constant speed；(3) after the perovskite precursor solution evaporation of substrate surface, perovskite thin film is formed in substrate surface.The perovskite thin film preparation method of the present invention has that preparation technology is easy, prepares that speed is fast, film quality is high, the uniform advantage of film thickness, large area, the perovskite photovoltaic device of scale preparation in great application prospect.
Description
Technical field
The invention belongs to field of photoelectric technology, and in particular to for the active light absorbing layer of Ca-Ti ore type photovoltaic device perovskite
Preparation method.
Background technology
In many novel renewable energies, solar power generation is undoubtedly most one of direction of prospect.With CH3NH3PbI3
For the hybrid inorganic-organic perovskite solar cell of representative, photoelectric transformation efficiency and relatively low system due to its protrusion
Standby cost, the great interest of domestic and international researcher was caused between nearly 5 years, and obtained development at full speed, at present the type sun
The efficiency of battery has broken through 22%, shows high application prospect.
Solution spin-coating method is the method for manufacturing thin film that mainly uses in the research of perovskite solar cell, have cost it is low,
The advantage that manipulation is simple and repeatability is high.However, prepared by the large area that the operational characteristic of spin coating technique in itself limits film
And mass production, seriously constrain its application in solar cell is commercially produced.In addition, solution spin coating technique is being made
There is relatively low perovskite precursor solution utilization rate (~5% or less) in standby process, also highlight economy it is low and
The disagreeableness deficiency of environment.Vapour deposition process is as a kind of physical deposition method, although the calcium titanium of high quality, large area can be realized
The preparation of ore deposit film, but preparation technology is complex, it is necessary to specific vacuum vapor deposition system, and prepare that speed is relatively low, material
Expect that utilization rate is limited, be also unfavorable for the prepare with scale of perovskite thin film and related device.Therefore, it is steady to develop large area, technique
Fixed and economic perovskite thin film technology of preparing is particularly important for the practical photovoltaic application towards perovskite thin film.Make
For one kind, fast and effectively method for manufacturing thin film, solution doctor blade technique are also introduced in the big face of perovskite thin film in recent years
In product, quick preparation.2014, the researcher such as Jen of Washington, DC university reports first prepared calcium titanium using knife coating
Ore deposit film, and realize being obviously improved for device photovoltaic performance and air stability.2017, Nebraska,USA university woods
The Jinsong Huang research groups in branch school are agreed by introducing mixed-cation technology, have been achieved with exceeding using knife coating
It is prepared by 18% Efficient devices.Due to superelevation utilization rate of raw materials of the knife coating when preparing film, and large area, low cost
With the unique advantage in terms of prepare with scale, this film preparing technology embodies greatly in the commercially producing of perovskite
Application potential.However, the perovskite thin film that at present prepared by knife coating need to be improved in terms of device repeatability, wherein, system
It is standby go out perovskite thin film uniformity it is relatively low be its technology stability major limiting bottleneck.
The content of the invention
It is an object of the invention to provide a kind of perovskite thin film fast preparation method based on brush techniques, solves current
Perovskite thin film has the problem of to be hoisted in terms of large area, process stabilizing and quick preparation.
The present invention is using brush techniques and combines the solvent engineering of precursor solution and regulates and controls, can effectively solve it is conventional scrape it is coated
Film thickness and the problem of uniformity controlling in journey, can be achieved large area, the one-step method of high quality perovskite thin film is quickly prepared,
Higher photoelectric transformation efficiency and device repetitive rate are also achieved in terms of photovoltaic application, before showing high commercial application
Scape.
It is a further object of the present invention to provide a kind of preparation technology of perovskite solar cell, the above-mentioned calcium of the technology utilization
The quick preparation method of titanium ore film prepares perovskite light absorbs active layer.
In order to achieve the above object, the invention provides a kind of quick side of preparation of perovskite thin film based on brush techniques
Method, including step：S1. perovskite precursor solution is prepared；S2. provide surface wettability good substrate；S3. heated in substrate
In the case of, the brush for being impregnated with perovskite precursor solution is brushed in substrate surface with constant speed；S4. it will brush and complete
Substrate continue to heat, vaporized precursor solvent is simultaneously annealed, and forms the perovskite thin film of well-crystallized.
In the present invention, described perovskite thin film fast preparation method, in the perovskite precursor solution described in step S1
PbI2Mol ratio with AI is 1:1, solution concentration is 0.5~2.5mol/L, and wherein A is CH3NH3 +With CH (NH2)2 +Cation
Arbitrary proportion mixes.
In the present invention, described perovskite thin film fast preparation method, perovskite precursor solution described in step S1
Solvent is by a kind of mixed solution with arbitrary proportion in DMF and DMSO or NMP, wherein described DMSO or NMP are in film
Play solvent engineering in preparation process, regulate and control perovskite nucleation density and rate of crystalline growth, lift thin film crystallization
Quality and uniformity.Wherein, described solvent engineering regulating and controlling effect has the characteristics that：(1) formed in precursor solution
PbI2- AI-X (X=DMSO or NMP) intermediate product, (2) can reduce nucleation density in film growth phase, promote large scale
The growth of perovskite crystal grain, typical grain size diameter are more than 1 micron.
Preferably, a kind of mixed proportion in DMF and DMSO or NMP is volume ratio 1:100-100:1.
In the present invention, described perovskite thin film fast preparation method, the good base of surface wettability described in step S2
Bottom, its purpose is to obtain good precursor solution infiltration and covering in substrate surface, be advantageous to be subsequently formed high surface
The perovskite thin film of coverage rate and high uniformity.In order to obtain higher wellability in substrate surface, can by thermal anneal process,
Ultra violet lamp, O2The methods of corona treatment, obtains.
In the present invention, described perovskite thin film fast preparation method, the brush described in step S3 is by cloth, fiber or dynamic
A kind of material in thing hair is made, and possesses following characteristics：(1) there is good wellability for precursor solution；(2) with
Substrate contact interface is smooth, and interface precursor solution is evenly distributed.
In the present invention, described perovskite thin film fast preparation method, during the brushing described in step S3, brush and base
Bottom directly contacts, and at the uniform velocity advances in the horizontal direction, it is preferred that gait of march 5-20mm/s；
In the present invention, described perovskite thin film fast preparation method, the brushing process described in step S3 is in horizontal heat
Carried out on plate, hot plate temperature keeps constant, it is preferred that hot plate heating-up temperature value is 60~160 DEG C；
In the present invention, described perovskite thin film fast preparation method, continue to heat described in step S3, it is preferred that add
The hot time is 5-30min, and temperature is 100~160 DEG C；
In the present invention, described perovskite thin film fast preparation method, preparing environment can be more in air, nitrogen, argon gas etc.
Implement in kind atmosphere, it is preferred that above-mentioned brushing process is carried out in air atmosphere, air humidity 10%-35%, temperature
For 20 DEG C -30 DEG C；
Compared with prior art, perovskite thin film fast preparation method of the invention, including at least following technique effect：
(1) it is thin more than 50 microns of perovskite can quickly to prepare crystal domain size in substrate previous step method for brushing process proposed by the present invention
Film, and film surface it is fine and close, it is smooth, without cavity blemish；(2) under the regulation and control of precursor solution solvent engineering, film crystal grain chi
It is very little to be more than 1 micron；(3) brush techniques proposed using the invention, the width of brush is adjusted, large area perovskite thin film can be achieved
Rapid one-step prepare；(4) brush techniques show very big application prospect in the preparation of scale perovskite thin film.
To reach above-mentioned purpose, present invention also offers a kind of preparation technology of perovskite solar cell, the technology utilization
The fast preparation method of above-mentioned perovskite thin film is prepared for the active light absorbing layer of perovskite solar cell, in device photovoltaic
Can on realize higher device photoelectric conversion efficiency.
In the preparation technology of above-mentioned perovskite solar cell, it is preferred that device architecture is carried by electro-conductive glass/fine and close electronics
Layer/mesoporous layer/calcium titanium ore bed/hole-conductive layer/metal electrode is taken to form, or by electro-conductive glass/hole-conductive layer/perovskite
Layer/electron extraction layer/metal electrode is formed.
The perovskite solar cell preparation technology of the present invention makes full use of brush techniques to be grown with reference to controllable film
Journey, a step process fast filming, preparation technology is simple, required equipment cost is cheap, and thin film crystallization quality is high, and is beneficial to big face
Product, the preparation of scale, great industrial prospect.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
Apply example to be used to explain the present invention together, be not construed as limiting the invention.
Fig. 1：The perovskite thin film low range SEM shape appearance figures prepared in embodiment 1；
Fig. 2：The perovskite thin film prepared in embodiment 1 is compared with high magnification SEM shape appearance figures；
Fig. 3：The perovskite thin film prepared in embodiment 1 is compared with the section SEM shape appearance figures under low range；
Embodiment
In order to thoroughly understand the present invention, detailed step and composition will be proposed in following description, in addition, many institutes are all
The composition or step known do not describe with details, to avoid causing the unnecessary limitation of the present invention.The preferable implementation of the present invention
Example is described in detail as follows, but in addition to these detailed descriptions, the present invention can also be implemented widely in other embodiments, and this
The scope of invention is not limited, and is defined by right.
Embodiment 1：
S1. perovskite precursor solution configures：By PbI2, MAI and DMSO press 1:1:1 mixed in molar ratio is in DMF solution
In, continuously stirred 1 hour under conditions of 70 DEG C of heating, be completely dissolved solute, be configured to PbI2The compound centres of-MAI-DMSO
The perovskite precursor solution of body, concentration 2mol/L；
S2. prepared by brush：Superfine fibre dust-free cloth is cut into 4cm is wide, the slice of 20cm length, connects in the same direction afterwards
Continuous folding for several times, is made the dustless cloth of 4cm*2cm sizes, clamps cloth along center with the wide stainless steel clips of 4cm, be prepared into
Brush, in preparation process, keep target head contacts face neatly smooth；
S3. substrate preparation and surface preparation：Will be by electro-conductive glass/fine and close TiO2Layer/mesoporous TiO2The substrate that layer is formed exists
Anneal 30 minutes under air atmosphere, 550 DEG C of temperature conditionss, substrate is transferred on 150 DEG C of hot plate after room temperature is down to；
S4. hot plate is kept for constant 150 DEG C, and it is molten that the brush prepared by non-dust cloth is fully infiltrated into perovskite precursor first
Liquid, then with basal edge side flat contact, brush substrate surface afterwards so that 10mm/s constant speed is horizontal.In this process
In, the contact angle of brush and substrate and contact dynamics and keep constant, perovskite precursor solution is in the case where substrate heats
The rapid perovskite thin film for crystallizing into uniform fold；
S5. the substrate that above-mentioned brushing is completed is continued to heat 10 minutes on hot plate.Above-mentioned preparation technology is in air atmosphere
Middle progress is enclosed, air humidity is maintained at~35%.
Embodiment 2：
S1. perovskite precursor solution configures：By PbI2, MAI and DMSO press 1:1:2 mixed in molar ratio is in DMF solution
In, continuously stirred 1 hour under conditions of 70 DEG C of heating, be completely dissolved solute, be configured to PbI2The compound centres of-MAI-DMSO
The perovskite precursor solution of body, concentration 2mol/L；
S2. prepared by brush：The animal origin for being derived from wolf hair brush is made to width about 4cm, thickness about 0.5cm flat type brush, used
Scissors repaiies the neat target contact interface for being located at brush top；
S3. substrate preparation and surface preparation：Will be by electro-conductive glass/fine and close TiO2Layer/mesoporous TiO2The substrate that layer is formed exists
Anneal 30 minutes under air atmosphere, 550 DEG C of temperature conditionss, substrate is transferred on 150 DEG C of hot plate after room temperature is down to；
S4. hot plate is kept for constant 150 DEG C, and it is molten that brush made of animal origin above-mentioned first fully infiltrates perovskite precursor
Liquid, the flatness of adjustment brush and target contact interface, then with basal edge side flat contact, afterwards with 10mm/s perseverance
Constant speed degree is horizontal to brush substrate surface.In the process, the contact angle of brush and substrate and contact dynamics and keep constant, calcium titanium
Ore deposit precursor solution crystallizes into rapidly the perovskite thin film of uniform fold in the case where substrate heats；
S5. the substrate that above-mentioned brushing is completed is continued to heat 10 minutes on hot plate.Above-mentioned preparation technology is in air atmosphere
Middle progress is enclosed, air humidity is maintained at~35%.
Embodiment 3：
S1. perovskite precursor solution configures：By PbI2, MAI and DMSO press 1:1:1 mixed in molar ratio is in DMF solution
In, continuously stirred 1 hour under conditions of 70 DEG C of heating, be completely dissolved solute, be configured to PbI2The compound centres of-MAI-DMSO
The perovskite precursor solution of body, concentration 2mol/L；
S2. prepared by brush：Superfine fibre dust-free cloth is cut into 5cm is wide, the slice of 20cm length, connects in the same direction afterwards
It is continuous to fold the dustless cloth that 5cm*2cm sizes are made, cloth is clamped along center with the wide stainless steel fixtures of 5cm, is prepared into brush,
In preparation process, keep target head contacts face neatly smooth；
S3., the stainless steel fixture of above-mentioned preparation is arranged on to the z-axis top of xyz D translation platforms, wherein on xy translational planes
The heating flat board of precise temperature control is integrated with, adjustment fixture makes brush made of above-mentioned superfine fibre dust-free cloth parallel with x/y plane；
S4. will be by electro-conductive glass/fine and close TiO2Layer/mesoporous TiO2The substrate that layer is formed is in air atmosphere, 550 DEG C of temperature strips
Annealed 30 minutes under part, substrate is transferred on the x/y plane heating flat board of D translation platform after room temperature is down to, heats flat board
150 DEG C of constant temperature are kept by temperature controller.Wherein size of foundation base is 5cm*6cm；
S5. perovskite precursor solution is directed to by brush position by liquid injecting pipeline, brush is fully infiltrated perovskite
Precursor solution；Contact distance of the brush with substrate is adjusted, makes brush and basal edge side flat contact, passes through control afterwards
Module moves translation stage, brush is moved horizontally with 10mm/s constant speed relative to substrate.In the process, in brush
The precursor solution of infiltration is uniformly applied to substrate surface, and the perovskite precursor solution smeared is in the case where substrate heats
The rapid perovskite thin film for crystallizing into uniform fold；
S6. the substrate that above-mentioned brushing is completed is continued to heat 10 minutes on heating flat board.Above-mentioned preparation technology exists
Carried out in air atmosphere, air humidity is maintained at~35%.
Embodiment 4：
S1. perovskite precursor solution configures：By PbI2, MAI and DMSO press 1:1:1 mixed in molar ratio is in DMF solution
In, continuously stirred 1 hour under conditions of 70 DEG C of heating, be completely dissolved solute, be configured to PbI2The compound centres of-MAI-DMSO
The perovskite precursor solution of body, concentration 2mol/L；
S2. prepared by brush：Superfine fibre dust-free cloth is cut into 4cm is wide, the slice of 20cm length, connects in the same direction afterwards
It is continuous to fold the dustless cloth that 4cm*2cm sizes are made, cloth is clamped along center with the wide stainless steel clips of 4cm, is prepared into brush,
In preparation process, keep target head contacts face neatly smooth；
S3. substrate preparation and surface preparation：Will be by electro-conductive glass/fine and close TiO2Layer/mesoporous TiO2The substrate that layer is formed exists
Anneal 30 minutes under air atmosphere, 550 DEG C of temperature conditionss, substrate is transferred on 150 DEG C of hot plate after room temperature is down to；
S4. hot plate is kept for constant 150 DEG C, first by~1ml precursor solution drop coating in the brush prepared by non-dust cloth
Surface, brush is fully infiltrated, it is horizontal with 10mm/s constant speed afterwards then by brush and basal edge side flat contact
Brush substrate surface.In the process, the contact angle of brush and substrate and contact dynamics and keep constant, before being infiltrated in brush
Body solution is uniformly applied to substrate surface, and the perovskite precursor solution smeared crystallizes rapidly in the case where substrate heats
Into the perovskite thin film of uniform fold；
S5. the substrate that above-mentioned brushing is completed is continued to heat 10 minutes on hot plate；Above-mentioned preparation technology is in air atmosphere
Middle progress is enclosed, air humidity is maintained at~35%；
S6. after substrate is down to room temperature, passed in the spin coating of perovskite thin film surface containing the hole of Spiro-OMeTAD and lithium salts
Defeated layer solution, spin-coating time 30 seconds, spin speed 4000rpm；
S7. the substrate for completing above-mentioned technique is placed in special metal mask plate, using electron beam evaporation process in table
Gold electrode thick face deposition 100nm, completes the preparation of perovskite solar cell device, wherein individual devices area is
0.11cm2。
The perovskite thin film fast preparation method using the present invention is can be seen that from Fig. 1 SEM shape appearance figures, can be achieved big
Effective preparation of area perovskite thin film, film are made up of large scale perovskite thin film domain, and film surface is uniform, smooth, nothing
Needle pore defect；Film is can be seen that from the more powerful SEM shape appearance figures of Fig. 2 to be made up of large scale perovskite crystal grain, surface
Smooth densification；From Fig. 3 a wide range of interior SEM sectional views can be seen that prepared perovskite thin film thickness uniformly, structure cause
It is close.The perovskite thin film prepared using the present invention also has good performance in Photovoltaic Device Performance, and structure system is just put with conventional
Standby perovskite solar cell device can realize average 16.00% device photoelectric conversion efficiency, and highest can realize 17.05%
Efficiency.
Claims (9)
1. a kind of preparation method of perovskite thin film, including step：
S1. perovskite precursor solution is prepared；Wherein, the solvent of described perovskite precursor solution be by DMF and DMSO or
A kind of mixed solution with arbitrary proportion in NMP；
S2. provide surface wettability good substrate；The good substrate of described surface wettability is that surface has meso-hole structure
Silicon chip, electro-conductive glass or polymer substrate, pass through to handle and obtain preferable surface wettability；
S3. in the case where substrate heats, the brush for being impregnated with perovskite precursor solution is brushed in substrate with constant speed
Surface；
S4. the substrate for brushing completion is continued to heat, vaporized precursor solvent is simultaneously annealed, and the perovskite for forming well-crystallized is thin
Film.
A kind of 2. preparation method of perovskite thin film according to claim 1, it is characterised in that described perovskite forerunner
PbI in liquid solution2Mol ratio with AI is 1:(0.8~1.2), wherein A are CH3NH3 +With CH (NH2)2 +Any ratio of cation
Example mixing, solution concentration is 0.5~2.5mol/L.
A kind of 3. preparation method of perovskite thin film according to claim 1, it is characterised in that described perovskite forerunner
The solvent of liquid solution is to be mixed by DMF with one kind in DMSO or NMP, and ratio is volume ratio 1:100-100:1.
4. the preparation method of a kind of perovskite thin film according to claim 1, it is characterised in that step S2 processing includes
Thermal anneal process or O2Corona treatment.
5. the preparation method of a kind of perovskite thin film according to claim 1, it is characterised in that described in step S3
Brush is made up of a kind of material in the good cloth of perovskite precursor solution wellability, fiber or animal hair, brush with
The target contact interface of substrate is smooth.
6. the preparation method of a kind of perovskite thin film according to claim 1, it is characterised in that described in step S3
During brushing, brush directly contacts with substrate, at the uniform velocity advances in the horizontal direction, gait of march 5-20mm/s.
7. the preparation method of a kind of perovskite thin film according to claim 1, it is characterised in that described in step S3
Brushing process is carried out on horizontal hot plate, and hot plate temperature keeps constant, and temperature value is 60~200 DEG C.
A kind of 8. preparation method of perovskite thin film according to claim 1, it is characterised in that in step S4, it is described after
The continuous heat time is 5-30min, and heating-up temperature is 70~150 DEG C.
A kind of 9. application of the preparation method of perovskite thin film according to any one of claim 1 to 8, for preparing calcium titanium
The active light absorbing layer of ore deposit solar cell.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766666A (en) * | 2018-06-07 | 2018-11-06 | 乐凯华光印刷科技有限公司 | A kind of low resistance, nano-silver thread transparent conductive film of high transparency and preparation method thereof |
| CN109449295A (en) * | 2018-10-30 | 2019-03-08 | 暨南大学 | Method for preparing perovskite film based on two-step printing |
| CN109545971A (en) * | 2018-11-16 | 2019-03-29 | 苏州大学 | A kind of preparation process of the perovskite solar battery using polyester fiber brush rubbing method |
| CN110289358A (en) * | 2019-06-11 | 2019-09-27 | 浙江浙能技术研究院有限公司 | A kind of perovskite film-forming process |
| CN111403613A (en) * | 2020-03-26 | 2020-07-10 | 武汉理工大学 | Method for preparing large-area semitransparent perovskite film by using scraper coating method and application thereof |
| WO2023184564A1 (en) * | 2022-03-30 | 2023-10-05 | 浙江大学 | Preparation method for nano-material macroscopic complex via substrate heating-solvent evaporation |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108766666A (en) * | 2018-06-07 | 2018-11-06 | 乐凯华光印刷科技有限公司 | A kind of low resistance, nano-silver thread transparent conductive film of high transparency and preparation method thereof |
| CN109449295A (en) * | 2018-10-30 | 2019-03-08 | 暨南大学 | Method for preparing perovskite film based on two-step printing |
| CN109449295B (en) * | 2018-10-30 | 2023-09-22 | 麦耀华 | Method for preparing perovskite film based on two-step printing |
| CN109545971A (en) * | 2018-11-16 | 2019-03-29 | 苏州大学 | A kind of preparation process of the perovskite solar battery using polyester fiber brush rubbing method |
| CN110289358A (en) * | 2019-06-11 | 2019-09-27 | 浙江浙能技术研究院有限公司 | A kind of perovskite film-forming process |
| CN111403613A (en) * | 2020-03-26 | 2020-07-10 | 武汉理工大学 | Method for preparing large-area semitransparent perovskite film by using scraper coating method and application thereof |
| WO2023184564A1 (en) * | 2022-03-30 | 2023-10-05 | 浙江大学 | Preparation method for nano-material macroscopic complex via substrate heating-solvent evaporation |
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Application publication date: 20180406 |