CN105428539A - Preparation method for perovskite solar cell absorption layer capable of improving photoelectric properties through controlling annealing pressure intensity atmosphere - Google Patents
Preparation method for perovskite solar cell absorption layer capable of improving photoelectric properties through controlling annealing pressure intensity atmosphere Download PDFInfo
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Abstract
The invention discloses a preparation method for a perovskite solar cell absorption layer capable of improving photoelectric properties through controlling an annealing pressure intensity atmosphere. The preparation method comprises the procedures: carrying out reagent preparing, carrying out cleaning, carrying out spin coating and carrying out annealing, i.e., firstly weighing methylamine iodine and lead iodide which are in the mole ratio of 3: 1, dissolving methylamine iodine and lead iodide in N,N-dimethylformamide in a mixed manner, and carrying out heating stirring for 10-14 hours at the temperature of 50-70 DEG C, so as to obtain a spin-coating solution for later use, wherein the mass fraction of N,N-dimethylformamide is 25-45%; fixing a substrate, which is cleaned until the substrate meets spin-coating requirements, and uniformly coating the substrate with 35-50 microliters of the spin-coating solution under nitrogen protection in a spin-coating manner, so as to obtain a uniform and stable coating film; carrying out annealing on the coating film attached substrate for 12-60 minutes at the temperature of 100-120 DEG C and the pressure of 4.5mTorr to 560Torr, and then, cooling the substrate to room temperature, thereby obtaining the target perovskite solar cell absorption layer. The perovskite solar cell absorption layer prepared by the method has the thickness of 200-500nm, and the electron mobility of the absorption layer is superior to that of absorption layers prepared by other methods, so that the efficiency of solar cells is increased.
Description
Technical field
The invention belongs to perovskite solar cell preparing technical field, be specifically related to a kind of when controlling to anneal pressure atmosphere improve the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties.
Background technology
The market share in solar cell market about 85% is occupied by crystal silicon solar energy battery, but the theoretical limit limited efficacy of crystalline silicon, just current, in crystal silicon solar energy battery, be difficult to obtain larger lifting again change.The shortcomings such as and its price is high, energy consumption reclaims slow, and preparation method is complicated, also constrain the development of photovoltaic industry greatly.Perovskite solar cell is the emerging solar cell of a class, mainly utilize the photovoltaic material with perovskite structure to realize opto-electronic conversion, it has, and raw material sources is extensive, structure is simple, price is low, can be prepared into the advantages such as flexible battery, is with a wide range of applications.
In recent years, organic-metallic-halide CH
3nH
3pbI
3, CH
3nH
3pbBr
3, CH
3nH
3pbCl
3, CH
3nH
3pbI
3-xcl
x, CH
3nH
3pbI
3-xbr
xdeng perovskite material because having the advantages such as the strong and band gap of long carrier transport distance, low exciton bind energy, optical absorption is adjustable, get more and more people's extensive concerning, its photoelectric conversion efficiency is ground from Miyasaka in 2009 3.8% of the group reported first that makes internal disorder or usurp and is brought up to 20.1% of report recently.It is allowed to set out towards the direction of industrialization gradually.
For improving device efficiency further, need to obtain the larger and smooth absorbed layer film of particle on the one hand; Wish that the perovskite thin film obtained has the absorption spectrum of relative broad range on the other hand.Current, perovskite absorbed layer is preparation method mainly contain: liquid phase method, gas phase assist liquid phase method, gas phase Co-evaporated Deposition method etc.Lead iodide becomes nanoscale perovskite tiny crystal grains with iodine methylamine Rapid self assembly in coating process, nucleation and coating growth direction are difficult to control, after film forming, in crystal, defect is more, regularity is poor, be difficult to form fine and close perovskite thin film, reduce the diffusion length of charge carrier, electron-hole pair compound is serious.Liquid phase method is subject to the various factors such as precursor solution component proportioning, concentration, solvent and spin coating rotating speed, crystalline quality is difficult to control, crystallization rear film pattern is different, and it is poor that reproducibility prepared by high-efficiency battery device, significantly limit perovskite-based solar cell industry process.
The present invention finds can control film growth, to obtain the absorbed layer film with different uniformity and thickness, particle diameter and different photoelectric properties by pressure during control absorbed layer annealing in process, atmosphere through repeatedly repeating to test.And current, do not have by short annealing and change atmosphere pressure and go the correlation technique improving these performances to be seen in report.Based on this, the present invention aims to provide one and carry out short annealing process to absorbed layer under the different pressure of different atmosphere, improve the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties, obtain the absorbed layer of different-thickness, different uniformity coefficient, different-grain diameter, different photoelectric properties, accelerate the industrialization process of perovskite solar cell.
Summary of the invention
The object of the present invention is to provide a kind of when controlling to anneal pressure atmosphere improve the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties.
The object of the present invention is achieved like this: described when controlling annealing pressure atmosphere improve the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties, comprise ingredients, clean, spin coating and annealing operation, specifically comprise:
A, ingredients: take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 25 ~ 45%: add thermal agitation 10 ~ 14h in 50 ~ 70 DEG C, obtains spin coating liquid for subsequent use;
B, clean: with cleaning agent, substrate to be cleaned, then with absolute ethyl alcohol and methyl alcohol, substrate is cleaned further respectively, finally use ultra violet lamp substrate, making substrate cleaning to meeting spin coating requirement;
35 ~ 50 μ l spin coating liquid, under nitrogen protection, are evenly spun on substrate, obtain uniform and stable film by C, spin coating: fixed by substrate;
D, annealing: will with the substrate of film in 100 ~ 120 DEG C, anneal under 4.5mTorr ~ 560Torr 12 ~ 60min, then be cooled to room temperature, aimed perovskite solar battery obsorbing layer.
The present invention proposes a kind of when controlling to anneal pressure atmosphere improve the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties.Anneal under being combined in different pressure atmosphere by spin-coating film and can obtain the perovskite absorbed layer of different-shape, different-grain diameter and optical property.And preparation condition can be adjusted as required, as spin coating rotating speed, time, annealing temperature and pressure etc., obtain the bustamentite methylamine absorbed layer film (CH with better film forming, optical property
3nH
3pbI
3), achieve the controllable variations of perovskite solar battery obsorbing layer crystal composition, size, pattern and absorbent properties, thus improve its stability and photoelectric properties.The thickness of the perovskite solar battery obsorbing layer adopting the method for the invention to prepare is 200 ~ 500nm, and electron mobility is obviously better than the obtained absorbed layer of additive method, improves the efficiency of solar cell, has application value.
Accompanying drawing explanation
Fig. 1 is the process chart of preparation method of the present invention.
Fig. 2 is the XRD collection of illustrative plates of perovskite solar battery obsorbing layer 100 ~ 120 DEG C time under different pressure after annealing in process 12 ~ 60min adopting the method for the invention to prepare.
Fig. 3 is the SEM collection of illustrative plates of perovskite solar battery obsorbing layer 100 ~ 120 DEG C time under different pressure after annealing in process 12 ~ 60min adopting the method for the invention to prepare, (a) 4.5mTorr, 120 DEG C, 12min, (b) 145mTorr, 120 DEG C, 12min, (c) 290mTorr, 120 DEG C, 12min, (d) 4Torr, 100 DEG C, 60min, (e) 560Torr, 100 DEG C, 60min, (f) cross section.
Fig. 4 is the absorption collection of illustrative plates of perovskite solar battery obsorbing layer 100 ~ 120 DEG C time under different pressure after annealing in process 12 ~ 60min adopting the method for the invention to prepare.
Embodiment
The present invention is further illustrated below, but limited the present invention never in any form, and any conversion done based on training centre of the present invention or replacement, all belong to protection scope of the present invention.
Of the present invention when controlling annealing pressure atmosphere improve the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties, comprise ingredients, clean, spin coating and annealing operation, specifically comprise:
Described ingredients operation refers to: take iodine methylamine and lead iodide that mol ratio is 3:1, and iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 25 ~ 45%: add thermal agitation 10 ~ 14h in 50 ~ 70 DEG C, obtains spin coating liquid for subsequent use.
Described cleaning process refers to: clean substrate with cleaning agent, then cleans further substrate with absolute ethyl alcohol and methyl alcohol respectively, finally uses ultra violet lamp substrate, makes substrate cleaning to meeting spin coating requirement.
Described spin coating operation refers to: fixed by substrate, under nitrogen protection, is evenly spun on substrate by 35 ~ 50 μ l spin coating liquid, obtains uniform and stable film;
Described annealing operation refers to: will with the substrate of film in 100 ~ 120 DEG C, and anneal under 4.5mTorr ~ 560Torr 12 ~ 60min, then be cooled to room temperature, aimed perovskite solar battery obsorbing layer.
Described in ingredients operation, the mol ratio of iodine methylamine and lead iodide is 3:1; Iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 40%.
Heating-up temperature described in ingredients operation is 60 DEG C; Mixing time is 12h.
Cleaning agent described in cleaning process is Common detergents, without particular/special requirement.
Cleaning further substrate with absolute ethyl alcohol and methyl alcohol described in cleaning process is adopt ultrasonic cleaning process.The frequency of described ultrasonic cleaning process is 50 ~ 55Hz; Scavenging period is 4 ~ 6min.
Use ultra violet lamp substrate described in cleaning process, irradiation time is 30min.
The rotating speed of spin coating described in spin coating operation is 2500 ~ 3200rpm; The time of spin coating is 38 ~ 42s; Spin coating liquid consumption is 40 ~ 45 μ l.
The temperature of annealing described in annealing operation is 100 ~ 120 DEG C; Pressure is 4.5mTorr, 145mTorr, 290mTorr, 4Torr, 560Torr; Time is 12 ~ 60min.
Described in clean, spin coating and annealing operation, substrate is transparent conductive film; Include but not limited to any one in ITO electro-conductive glass, FTO electro-conductive glass or simple glass.
The thickness of described perovskite solar battery obsorbing layer is 200 ~ 500nm.
embodiment 1
Take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 25%, puts into glove box and fully stirs 12h in 60 DEG C with magnetic stirring apparatus, obtains bustamentite methylamine spin coating liquid for subsequent use.Select ITO electro-conductive glass as substrate, first with cleaning agent, substrate cleaned, more respectively with absolute ethyl alcohol and methyl alcohol by substrate in the ultrasonic lower each cleaning 5min of 53Hz, finally using ultra violet lamp substrate 30min, making substrate cleaning to meeting spin coating requirement.Substrate is put into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with the rotating speed spin coating 40s of 3000rpm, 45 μ l spin coating liquid are evenly spun on substrate, obtain uniform and stable film.Put into quick anneal oven by with the substrate of film, in 120 DEG C, 4.5mTorr(and vacuum) under to anneal 12min, then naturally cool to room temperature, aimed perovskite solar battery obsorbing layer.
It is bustamentite methylamine that the XRD collection of illustrative plates that in Fig. 2, this embodiment is corresponding shows this perovskite solar battery obsorbing layer, and the crystal face corresponding to each peak is respectively (110), (220), (224), (404); In addition, the peak of lead iodide is also had, but more weak.The SEM that Fig. 3 (a) is this embodiment schemes, and absorbed layer particle is comparatively large as can be seen from Figure, and uniformity is better.The absorption collection of illustrative plates that in Fig. 4, this embodiment is corresponding shows this perovskite solar battery obsorbing layer all has stronger absorption in whole visible-range, describes the photoelectric properties that it is good; And arrive influx and translocation in 500nm wave band 300, be more suitable for special operation under this wave band.
embodiment 2
Take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 25%, puts into glove box and fully stirs 14h in 50 DEG C with magnetic stirring apparatus, obtains bustamentite methylamine spin coating liquid for subsequent use.Select ITO electro-conductive glass as substrate, first with cleaning agent, substrate cleaned, more respectively with absolute ethyl alcohol and methyl alcohol by substrate in the ultrasonic lower each cleaning 4min of 55Hz, finally using ultra violet lamp substrate 30min, making substrate cleaning to meeting spin coating requirement.Substrate is put into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with the rotating speed spin coating 38s of 3200rpm, 40 μ l spin coating liquid are evenly spun on substrate, obtain uniform and stable film.Put into quick anneal oven by with the substrate of film, in 120 DEG C, anneal under 145mTorr 12min, then naturally cool to room temperature, aimed perovskite solar battery obsorbing layer.
It is bustamentite methylamine that the XRD collection of illustrative plates that in Fig. 2, this embodiment is corresponding shows this perovskite solar battery obsorbing layer, and the crystal face corresponding to each peak is respectively (110), (220), (224), (404); In addition, the peak of lead iodide is also had, more by force.The SEM that Fig. 3 (b) is this embodiment schemes, and absorbed layer particle is comparatively large as can be seen from Figure, and uniformity is better.The absorption collection of illustrative plates that in Fig. 4, this embodiment is corresponding shows this perovskite solar battery obsorbing layer all has stronger absorption in whole visible-range, describes the photoelectric properties that it is good.
embodiment 3
Take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 25%, puts into glove box and fully stirs 10h in 70 DEG C with magnetic stirring apparatus, obtains bustamentite methylamine spin coating liquid for subsequent use.Select FTO electro-conductive glass as substrate, first with cleaning agent, substrate cleaned, more respectively with absolute ethyl alcohol and methyl alcohol by substrate in the ultrasonic lower each cleaning 6min of 50Hz, finally using ultra violet lamp substrate 30min, making substrate cleaning to meeting spin coating requirement.Substrate is put into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with the rotating speed spin coating 42s of 2500rpm, 50 μ l spin coating liquid are evenly spun on substrate, obtain uniform and stable film.Put into quick anneal oven by with the substrate of film, in 120 DEG C, anneal under 290mTorr 12min, then naturally cool to room temperature, aimed perovskite solar battery obsorbing layer.
It is bustamentite methylamine that the XRD collection of illustrative plates that in Fig. 2, this embodiment is corresponding shows this perovskite solar battery obsorbing layer, and the crystal face corresponding to each peak is respectively (110), (220), (224), (404); In addition, also have the peak of lead iodide, intensity is stronger.The SEM that Fig. 3 (c) is this embodiment schemes, and absorbed layer particle is comparatively large as can be seen from Figure, and uniformity is better.The absorption collection of illustrative plates that in Fig. 4, this embodiment is corresponding shows this perovskite solar battery obsorbing layer all has stronger absorption in whole visible-range, describes the photoelectric properties that it is good.
embodiment 4
Take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 40%, puts into glove box and fully stirs 11h in 60 DEG C with magnetic stirring apparatus, obtains bustamentite methylamine spin coating liquid for subsequent use.Select FTO electro-conductive glass as substrate, first with cleaning agent, substrate cleaned, more respectively with absolute ethyl alcohol and methyl alcohol by substrate in the ultrasonic lower each cleaning 5min of 53Hz, finally using ultra violet lamp substrate 30min, making substrate cleaning to meeting spin coating requirement.Substrate is put into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with the rotating speed spin coating 40s of 2800rpm, 40 μ l spin coating liquid are evenly spun on substrate, obtain uniform and stable film.Put into quick anneal oven by with the substrate of film, in 100 DEG C, anneal under 4Torr 60min, then naturally cool to room temperature, aimed perovskite solar battery obsorbing layer.
It is bustamentite methylamine that the XRD collection of illustrative plates that in Fig. 2, this embodiment is corresponding shows this perovskite solar battery obsorbing layer, and the crystal face corresponding to each peak is respectively (110), (220), (314), wherein (110), (220) face is the strongest, (224), the peak in (404) face disappears; In addition, the peak of lead iodide is also had, but more weak.The SEM that Fig. 3 (d) is this embodiment schemes, and absorbed layer particle is comparatively large as can be seen from Figure, and uniformity is better.The absorption collection of illustrative plates that in Fig. 4, this embodiment is corresponding shows this perovskite solar battery obsorbing layer all has stronger absorption in whole visible-range, describes the photoelectric properties that it is good; And arrive influx and translocation in 800nm wave band 500, be more suitable for special operation under this wave band.
embodiment 5
Take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 38%, puts into glove box and fully stirs 13h in 55 DEG C with magnetic stirring apparatus, obtains bustamentite methylamine spin coating liquid for subsequent use.Select FTO electro-conductive glass as substrate, first with cleaning agent, substrate cleaned, more respectively with absolute ethyl alcohol and methyl alcohol by substrate in the ultrasonic lower each cleaning 5min of 53Hz, finally using ultra violet lamp substrate 30min, making substrate cleaning to meeting spin coating requirement.Substrate is put into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with the rotating speed spin coating 40s of 3000rpm, 48 μ l spin coating liquid are evenly spun on substrate, obtain uniform and stable film.Put into quick anneal oven by with the substrate of film, in 100 DEG C, anneal under 560Torr 60min, then naturally cool to room temperature, aimed perovskite solar battery obsorbing layer.
It is bustamentite methylamine that the XRD collection of illustrative plates that in Fig. 2, this embodiment is corresponding shows this perovskite solar battery obsorbing layer, and the crystal face corresponding to each peak is respectively (110), (220), (314), wherein (110), (220) face is the strongest, (224), the peak in (404) face disappears; In addition, the peak of lead iodide is also had, but more weak.The SEM that Fig. 3 (e) is this embodiment schemes, and absorbed layer particle is comparatively large as can be seen from Figure, and uniformity is better.The absorption collection of illustrative plates that in Fig. 4, this embodiment is corresponding shows this perovskite solar battery obsorbing layer all has stronger absorption in whole visible-range, describes the photoelectric properties that it is good.Prepare close under atmospheric pressure, condition more easily realizes, but compared with the absorbent properties under other conditions almost.
Claims (10)
1. when controlling to anneal, pressure atmosphere improves a preparation method for the perovskite solar battery obsorbing layer of its photoelectric properties, it is characterized in that comprising ingredients, clean, spin coating and annealing operation, specifically comprises:
A, ingredients: take iodine methylamine and lead iodide that mol ratio is 3:1, iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 25 ~ 45%: add thermal agitation 10 ~ 14h in 50 ~ 70 DEG C, obtains spin coating liquid for subsequent use;
B, clean: with cleaning agent, substrate to be cleaned, then with absolute ethyl alcohol and methyl alcohol, substrate is cleaned further respectively, finally use ultra violet lamp substrate, making substrate cleaning to meeting spin coating requirement;
35 ~ 50 μ l spin coating liquid, under nitrogen protection, are evenly spun on substrate, obtain uniform and stable film by C, spin coating: fixed by substrate;
D, annealing: will with the substrate of film in 100 ~ 120 DEG C, anneal under 4.5mTorr ~ 560Torr 12 ~ 60min, then be cooled to room temperature, aimed perovskite solar battery obsorbing layer.
2. preparation method according to claim 1, is characterized in that the mol ratio of iodine methylamine and lead iodide described in operation A is 3:1; Iodine methylamine, lead iodide mixing are dissolved in DMF, and its mass fraction is 40%.
3. preparation method according to claim 1, is characterized in that heating-up temperature described in operation A is 60 DEG C; Mixing time is 12h.
4. preparation method according to claim 1, is characterized in that cleaning further substrate with absolute ethyl alcohol and methyl alcohol described in process B is adopt ultrasonic cleaning process.
5. preparation method according to claim 4, is characterized in that the frequency of ultrasonic cleaning process described in process B is 50 ~ 55Hz; Scavenging period is 4 ~ 6min.
6. preparation method according to claim 1, is characterized in that using ultra violet lamp substrate described in process B, and irradiation time is 30min.
7. preparation method according to claim 1, is characterized in that the rotating speed of spin coating described in operation C is 2500 ~ 3200rpm; The time of spin coating is 38 ~ 42s; Spin coating liquid consumption is 40 ~ 45 μ l.
8. preparation method according to claim 1, is characterized in that the temperature of annealing described in step D is 100 ~ 120 DEG C; Pressure is 4.5mTorr, 145mTorr, 290mTorr, 4Torr, 560Torr; Time is 12 ~ 60min.
9. preparation method according to claim 1, is characterized in that substrate described in process B, C, D is transparent conductive film.
10. preparation method according to claim 9, is characterized in that substrate described in process B, C, D is any one in ITO electro-conductive glass, FTO electro-conductive glass or simple glass.
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CN106119971A (en) * | 2016-07-06 | 2016-11-16 | 福州大学 | The preparation of a kind of organic-inorganic perovskite spike crystal and application thereof |
CN111403610A (en) * | 2020-03-19 | 2020-07-10 | 武汉理工大学 | High-performance organic-inorganic hybrid perovskite photoelectric material and preparation method and application thereof |
CN111435707A (en) * | 2019-07-10 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Method for improving film forming quality of perovskite thin film and perovskite solar cell |
CN112186109A (en) * | 2020-09-24 | 2021-01-05 | 南京大学 | Perovskite thin film preparation method, perovskite thin film and perovskite solar cell |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106119971A (en) * | 2016-07-06 | 2016-11-16 | 福州大学 | The preparation of a kind of organic-inorganic perovskite spike crystal and application thereof |
CN111435707A (en) * | 2019-07-10 | 2020-07-21 | 杭州纤纳光电科技有限公司 | Method for improving film forming quality of perovskite thin film and perovskite solar cell |
CN111435707B (en) * | 2019-07-10 | 2022-09-23 | 杭州纤纳光电科技有限公司 | Method for improving film forming quality of perovskite thin film and perovskite solar cell |
CN111403610A (en) * | 2020-03-19 | 2020-07-10 | 武汉理工大学 | High-performance organic-inorganic hybrid perovskite photoelectric material and preparation method and application thereof |
CN112186109A (en) * | 2020-09-24 | 2021-01-05 | 南京大学 | Perovskite thin film preparation method, perovskite thin film and perovskite solar cell |
CN112186109B (en) * | 2020-09-24 | 2023-12-12 | 南京大学 | Perovskite thin film preparation method, perovskite thin film and perovskite solar cell |
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