CN105428539B - Pressure atmosphere improves the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties during a kind of control annealing - Google Patents
Pressure atmosphere improves the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties during a kind of control annealing Download PDFInfo
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Abstract
The preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties is improved the invention discloses pressure atmosphere during a kind of control annealing.The preparation method includes ingredients, cleaning, spin coating and annealing operation, weighs mol ratio first as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, in N dimethylformamides, its mass fraction is 25 ~ 45%：It is standby that spin coating liquid is obtained after 50 ~ 70 DEG C of 10 ~ 14h of heating stirring.Cleaning to the substrate for meeting spin coating requirement is fixed, under nitrogen protection, 35 ~ 50 μ l spin coatings liquid is uniformly spun on substrate, obtain uniform and stable film.By the substrate with film in 100 ~ 120 DEG C, anneal 12 ~ 60min under 4.5mTorr ~ 560Torr, is cooled to room temperature, you can obtains aimed perovskite solar battery obsorbing layer.Using perovskite solar battery obsorbing layer thickness prepared by methods described, electron mobility is better than absorbed layer made from other method, improves solar battery efficiency for 200 ~ 500nm.
Description
Technical field
The invention belongs to perovskite solar cell preparing technical field, and in particular to pressure atmosphere during one kind control annealing
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 pole of crystalline silicon
Limited efficacy is limited, is difficult to obtain larger lifting again to change in terms of crystal silicon solar energy battery at present.And it
Price is high, and energy consumption recovery is slow, the shortcomings of preparation method complexity, also constrains the development of photovoltaic industry significantly.The perovskite sun
Energy battery is a kind of emerging solar cell, mainly realizes that photoelectricity turns using the photovoltaic material with perovskite structure
Change, it has the advantages that raw material sources are extensive, simple in construction, price is low, can be prepared into flexible battery, has a wide range of applications
Prospect.
In recent years, organic-metallic-halide CH3NH3PbI3、CH3NH3PbBr3、CH3NH3PbCl3、CH3NH3PbI3-xClx、
CH3NH3PbI3-xBrxDeng perovskite material because strong with long carrier transport distance, low exciton bind energy, optical absorption
And the advantages such as band gap is adjustable, get more and more people's extensive concerning, its photoelectric transformation efficiency was ground from Miyasaka in 2009 makes internal disorder or usurp group first
The 3.8% of report brings up to 20.1% reported recently.It is allowed to be seted out progressively towards the direction of industrialization.
Further to improve device efficiency, on the one hand need to obtain the larger and smooth absorption layer film of particle；The opposing party
The perovskite thin film that face is intentionally got has the absorption spectrum of relative broad range.Currently, perovskite absorbed layer preparation method mainly has：
Liquid phase method, gas phase auxiliary liquid phase method, gas phase Co-evaporated Deposition method etc..Lead iodide and iodine the methylamine Rapid self assembly in coating process
Into nanoscale perovskite tiny crystal grains, nucleation and coating growth direction are difficult to control, and defect is more in crystal after film forming, rule
Whole degree is poor, it is difficult to forms the perovskite thin film of densification, reduces the diffusion length of carrier, electron-hole pair is compound serious.Liquid
Phase method is influenceed by many factors such as precursor solution component proportioning, concentration, solvent and spin coating rotating speeds, and crystalline quality is difficult to control
System, crystallization rear film pattern is different, and high-efficiency battery device preparation reproducibility is poor, significantly limit perovskite-based solar energy
Battery industry process.
Pressure, atmosphere when the present invention has found to make annealing treatment by controlling absorbed layer through multiplicating experiment can control thin
Film grows, to obtain having the absorption layer film of different uniformities and thickness, particle diameter and different photoelectric properties.And working as
Before, do not have by short annealing and change atmosphere pressure and go the correlation technique for improving these performances to be seen in report.Based on this, this
Invention aims to provide one kind and carries out short annealing processing to absorbed layer under different atmosphere difference pressure, improves its photoelectric properties
The preparation method of perovskite solar battery obsorbing layer, obtain different-thickness, different uniformity coefficients, different-grain diameter, different photoelectricity
The absorbed layer of performance, accelerate the industrialization process of perovskite solar cell.
The content of the invention
It is an object of the invention to provide the perovskite sun that pressure atmosphere during a kind of control annealing improves its photoelectric properties
The preparation method of energy battery obsorbing layer.
The object of the present invention is achieved like this：Pressure atmosphere improves the perovskite of its photoelectric properties during the control annealing
The preparation method of solar battery obsorbing layer, including ingredients, cleaning, spin coating and annealing operation, are specifically included：
A, ingredients：Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- bis-
NMF, its mass fraction are 25 ~ 45%：In 50 ~ 70 DEG C of 10 ~ 14h of heating stirring, it is standby to obtain spin coating liquid；
B, clean：Substrate is cleaned with cleaning agent, then respectively with absolute ethyl alcohol and methanol to the further cleaning of substrate,
Ultra violet lamp substrate is finally used, makes substrate cleaning to meeting spin coating requirement；
C, spin coating：Substrate is fixed, under nitrogen protection, 35 ~ 50 μ l spin coatings liquid is uniformly spun on substrate, obtained uniformly
Stable film；
D, anneal：By the substrate with film in 100 ~ 120 DEG C, anneal 12 ~ 60 min under 4.5mTorr ~ 560Torr, then
It is cooled to room temperature, you can obtain aimed perovskite solar battery obsorbing layer.
The present invention proposes the perovskite solar cell that a kind of pressure atmosphere when controlling annealing improves its photoelectric properties and inhaled
Receive the preparation method of layer.Different-shape, different-grain diameter can be obtained by being incorporated in annealing under different pressure atmosphere by spin-coating film
And the perovskite absorbed layer of optical property.And preparation condition can be adjusted as needed, such as spin coating rotating speed, time, annealing temperature
And pressure etc., obtain that there is the bustamentite methylamine of preferable film forming, optical property to absorb layer film（CH3NH3PbI3）, realize calcium
Titanium ore solar battery obsorbing layer crystal composition, size, the controllable variations of pattern and absorbent properties, so as to improve its stability
And photoelectric properties.The thickness of the perovskite solar battery obsorbing layer of the method for the invention preparation is used as 200 ~ 500nm, electricity
Transport factor is substantially better than absorbed layer made from other method, improves the efficiency of solar cell, great application value.
Brief description of the drawings
Fig. 1 is the process chart of preparation method of the present invention.
Fig. 2 is the perovskite solar battery obsorbing layer prepared using the method for the invention difference at 100 ~ 120 DEG C
The XRD spectrum after 12 ~ 60min is made annealing treatment under pressure.
Fig. 3 is the perovskite solar battery obsorbing layer prepared using the method for the invention difference at 100 ~ 120 DEG C
The SEM spectrum after 12 ~ 60 min is made annealing treatment under pressure,（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）
Section.
Fig. 4 is the perovskite solar battery obsorbing layer prepared using the method for the invention difference at 100 ~ 120 DEG C
The absorption collection of illustrative plates after 12 ~ 60min is made annealing treatment under pressure.
Embodiment
The present invention is further illustrated below, but the present invention is not any limitation as in any way, based on the present invention
Any conversion or replacement that training centre is made, belong to protection scope of the present invention.
Pressure atmosphere improves the perovskite solar battery obsorbing layer of its photoelectric properties during control annealing of the present invention
Preparation method, including ingredients, cleaning, spin coating and annealing operation, are specifically included：
The ingredients process refers to：Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed
DMF is dissolved in, its mass fraction is 25 ~ 45%：In 50 ~ 70 DEG C of 10 ~ 14h of heating stirring, it is standby to obtain spin coating liquid.
The cleaning process refers to：Substrate is cleaned with cleaning agent, then respectively with absolute ethyl alcohol and methanol to substrate
Further cleaning, finally with ultra violet lamp substrate, make substrate cleaning to meeting spin coating requirement.
The spin coating process refers to：Substrate is fixed, under nitrogen protection, 35 ~ 50 μ l spin coatings liquid are uniformly spun on lining
On bottom, uniform and stable film is obtained；
The annealing operation refers to：Substrate with film is annealed 12 under 100 ~ 120 DEG C, 4.5mTorr ~ 560Torr
~ 60min, is cooled to room temperature, you can obtains aimed perovskite solar battery obsorbing layer.
The mol ratio of iodine methylamine and lead iodide described in ingredients process is 3：1；Iodine methylamine, lead iodide are mixed and are dissolved in N, N- bis-
NMF, its mass fraction are 40%.
Heating-up temperature described in ingredients process is 60 DEG C；Mixing time is 12h.
Cleaning agent described in cleaning process is Common detergents, no particular/special requirement.
Described in cleaning process with absolute ethyl alcohol and methanol it is further to substrate cleaning be to use ultrasonic cleaning process.It is described super
The frequency of sound wave ablution is 50 ~ 55Hz；Scavenging period is 4 ~ 6min.
Ultra violet lamp substrate, irradiation time 30min are used described in cleaning process.
The rotating speed of spin coating described in spin coating process is 2500 ~ 3200rpm；The time of spin coating is 38 ~ 42s；Spin coating liquid dosage is
40~45μl。
The temperature annealed described in annealing operation is 100 ~ 120 DEG C；Pressure be 4.5mTorr, 145mTorr, 290mTorr,
4Torr、560Torr；Time is 12 ~ 60min.
Cleaning, spin coating and substrate described in annealing operation are transparent conductive film；Including but not limited to ITO electro-conductive glass, FTO
Any of electro-conductive glass or simple glass.
The thickness of the perovskite solar battery obsorbing layer is 200 ~ 500nm.
Embodiment 1
Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- dimethyl formyls
Amine, its mass fraction are 25%, are put into glove box and are sufficiently stirred 12h with magnetic stirring apparatus in 60 DEG C, obtain bustamentite methylamine spin coating liquid
It is standby.ITO electro-conductive glass is selected to be cleaned first with cleaning agent to substrate, then use absolute ethyl alcohol and first respectively as substrate
Alcohol each cleaning 5min under 53Hz ultrasounds by substrate, finally with ultra violet lamp substrate 30min, make substrate cleaning to meeting spin coating
It is required that.Place the substrate into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with turning for 3000rpm
Fast spin coating 40s, 45 μ l spin coatings liquid are uniformly spun on substrate, obtain uniform and stable film.Substrate with film is put into
In quick anneal oven, in 120 DEG C, 4.5mTorr（That is vacuum）Lower annealing 12min, then naturally cool to room temperature, you can obtain target
Perovskite solar battery obsorbing layer.
XRD spectrum corresponding to the embodiment shows that the perovskite solar battery obsorbing layer is bustamentite methylamine in Fig. 2, each peak
Corresponding crystal face is respectively（110）,（220）,（224）,（404）；In addition, the also peak of lead iodide, but weaker.Fig. 3（a）For
The SEM figures of the embodiment, absorbed layer particle is larger as can be seen from Figure, and uniformity is preferable.Figure is absorbed in Fig. 4 corresponding to the embodiment
Spectrum shows that the perovskite solar battery obsorbing layer has stronger absorption in whole visible-range, illustrates that it is good
Photoelectric properties；And the influx and translocation in 300 to 500nm wave bands, it is more suitable for the special operation under the wave band.
Embodiment 2
Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- dimethyl formyls
Amine, its mass fraction are 25%, are put into glove box and are sufficiently stirred 14h with magnetic stirring apparatus in 50 DEG C, obtain bustamentite methylamine spin coating liquid
It is standby.ITO electro-conductive glass is selected to be cleaned first with cleaning agent to substrate, then use absolute ethyl alcohol and first respectively as substrate
Alcohol each cleaning 4min under 55Hz ultrasounds by substrate, finally with ultra violet lamp substrate 30min, make substrate cleaning to meeting spin coating
It is required that.Place the substrate into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with turning for 3200rpm
Fast spin coating 38s, 40 μ l spin coatings liquid are uniformly spun on substrate, obtain uniform and stable film.Substrate with film is put into
In quick anneal oven, anneal 12min under 120 DEG C, 145mTorr, then naturally cools to room temperature, you can obtains aimed perovskite too
Positive energy battery obsorbing layer.
XRD spectrum corresponding to the embodiment shows that the perovskite solar battery obsorbing layer is bustamentite methylamine in Fig. 2, each peak
Corresponding crystal face is respectively（110）,（220）,（224）,（404）；In addition, the also peak of lead iodide, more by force.Fig. 3（b）For this
The SEM figures of embodiment, absorbed layer particle is larger as can be seen from Figure, and uniformity is preferable.Collection of illustrative plates is absorbed in Fig. 4 corresponding to the embodiment
Show that the perovskite solar battery obsorbing layer has stronger absorption in whole visible-range, illustrate its good light
Electrical property.
Embodiment 3
Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- dimethyl formyls
Amine, its mass fraction are 25%, are put into glove box and are sufficiently stirred 10h with magnetic stirring apparatus in 70 DEG C, obtain bustamentite methylamine spin coating liquid
It is standby.FTO electro-conductive glass is selected to be cleaned first with cleaning agent to substrate, then use absolute ethyl alcohol and first respectively as substrate
Alcohol each cleaning 6min under 50Hz ultrasounds by substrate, finally with ultra violet lamp substrate 30min, make substrate cleaning to meeting spin coating
It is required that.Place the substrate into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with turning for 2500rpm
Fast spin coating 42s, 50 μ l spin coatings liquid are uniformly spun on substrate, obtain uniform and stable film.Substrate with film is put into
In quick anneal oven, anneal 12min under 120 DEG C, 290mTorr, then naturally cools to room temperature, you can obtains aimed perovskite too
Positive energy battery obsorbing layer.
XRD spectrum corresponding to the embodiment shows that the perovskite solar battery obsorbing layer is bustamentite methylamine in Fig. 2, each peak
Corresponding crystal face is respectively（110）,（220）,（224）,（404）；In addition, also the peak of lead iodide, intensity are stronger.Fig. 3（c）
Scheme for the SEM of the embodiment, absorbed layer particle is larger as can be seen from Figure, and uniformity is preferable.Absorbed in Fig. 4 corresponding to the embodiment
Collection of illustrative plates shows that the perovskite solar battery obsorbing layer has stronger absorption in whole visible-range, illustrates that its is good
Photoelectric properties.
Embodiment 4
Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- dimethyl formyls
Amine, its mass fraction are 40%, are put into glove box and are sufficiently stirred 11h with magnetic stirring apparatus in 60 DEG C, obtain bustamentite methylamine spin coating liquid
It is standby.FTO electro-conductive glass is selected to be cleaned first with cleaning agent to substrate, then use absolute ethyl alcohol and first respectively as substrate
Alcohol each cleaning 5min under 53Hz ultrasounds by substrate, finally with ultra violet lamp substrate 30min, make substrate cleaning to meeting spin coating
It is required that.Place the substrate into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with turning for 2800rpm
Fast spin coating 40s, 40 μ l spin coatings liquid are uniformly spun on substrate, obtain uniform and stable film.Substrate with film is put into
In quick anneal oven, anneal 60min under 100 DEG C, 4Torr, then naturally cools to room temperature, you can obtains aimed perovskite solar energy
Battery obsorbing layer.
XRD spectrum corresponding to the embodiment shows that the perovskite solar battery obsorbing layer is bustamentite methylamine in Fig. 2, each peak
Corresponding crystal face is respectively（110）,（220）,（314）, wherein（110）,（220）Face is most strong,（224）,（404）The peak in face disappears
Lose；In addition, the also peak of lead iodide, but weaker.Fig. 3（d）For the embodiment SEM scheme, as can be seen from Figure absorbed layer particle compared with
Greatly, uniformity is preferable.Collection of illustrative plates is absorbed in Fig. 4 corresponding to the embodiment and shows that the perovskite solar battery obsorbing layer entirely may be used
Seeing has stronger absorption in optical range, illustrate its good photoelectric properties；And the influx and translocation in 500 to 800nm wave bands,
It is more suitable for the special operation under the wave band.
Embodiment 5
Mol ratio is weighed as 3：1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- dimethyl formyls
Amine, its mass fraction are 38%, are put into glove box and are sufficiently stirred 13h with magnetic stirring apparatus in 55 DEG C, obtain bustamentite methylamine spin coating liquid
It is standby.FTO electro-conductive glass is selected to be cleaned first with cleaning agent to substrate, then use absolute ethyl alcohol and first respectively as substrate
Alcohol each cleaning 5min under 53Hz ultrasounds by substrate, finally with ultra violet lamp substrate 30min, make substrate cleaning to meeting spin coating
It is required that.Place the substrate into the glove box under nitrogen atmosphere, be fixed on spin coater, under nitrogen protection, with turning for 3000rpm
Fast spin coating 40s, 48 μ l spin coatings liquid are uniformly spun on substrate, obtain uniform and stable film.Substrate with film is put into
In quick anneal oven, anneal 60min under 100 DEG C, 560Torr, then naturally cools to room temperature, you can obtains the aimed perovskite sun
Can battery obsorbing layer.
XRD spectrum corresponding to the embodiment shows that the perovskite solar battery obsorbing layer is bustamentite methylamine in Fig. 2, each peak
Corresponding crystal face is respectively（110）,（220）,（314）, wherein（110）,（220）Face is most strong,（224）,（404）The peak in face disappears
Lose；In addition, the also peak of lead iodide, but weaker.Fig. 3（e）For the embodiment SEM scheme, as can be seen from Figure absorbed layer particle compared with
Greatly, uniformity is preferable.Collection of illustrative plates is absorbed in Fig. 4 corresponding to the embodiment and shows that the perovskite solar battery obsorbing layer entirely may be used
Seeing has stronger absorption in optical range, illustrate its good photoelectric properties.Prepared under close to atmospheric pressure, condition is easier
Realize, but compared with the absorbent properties under other conditions almost.
Claims (10)
1. pressure atmosphere improves the preparation method of the perovskite solar battery obsorbing layer of its photoelectric properties during a kind of control annealing,
It is characterized in that including ingredients, cleaning, spin coating and annealing operation, specifically include：
A, ingredients：Mol ratio is weighed as 3:1 iodine methylamine and lead iodide, iodine methylamine, lead iodide are mixed and are dissolved in N, N- dimethyl
Formamide, its mass fraction are 25 ~ 45%；Spin coating liquid is obtained in 50 ~ 70 DEG C of 10 ~ 14h of heating stirring, it is standby；
B, clean：Substrate is cleaned with cleaning agent, then respectively with absolute ethyl alcohol and methanol to the further cleaning of substrate, finally
With ultra violet lamp substrate, make substrate cleaning to meeting spin coating requirement；
C, spin coating：Substrate is fixed, under nitrogen protection, 35 ~ 50 μ l spin coatings liquid is uniformly spun on substrate, obtained uniform and stable
Film；
D, anneal：By the substrate with film in 100 ~ 120 DEG C, anneal 12 ~ 60min under 4.5mTorr ~ 560Torr, then cools down
To room temperature, aimed perovskite solar battery obsorbing layer is obtained.
2. preparation method according to claim 1, it is characterised in that mass fraction is 40% in process A.
3. preparation method according to claim 1, it is characterised in that process A is in 60 DEG C of heating stirring 12h.
4. preparation method according to claim 1, it is characterised in that one is entered to substrate with absolute ethyl alcohol and methanol described in process B
It is ultrasonic cleaning process to walk cleaning.
5. preparation method according to claim 4, it is characterised in that the frequency of the ultrasonic cleaning process is 50 ~ 55Hz, clearly
It is 4 ~ 6min to wash the time.
6. preparation method according to claim 1, it is characterised in that the irradiation time of ultra violet lamp substrate is used described in process B
For 30min.
7. preparation method according to claim 1, it is characterised in that the rotating speed of spin coating described in process C be 2500 ~ 3200rpm,
Spin-coating time is 38 ~ 42s, spin coating liquid dosage is 40 ~ 45 μ l.
8. preparation method according to claim 1, it is characterised in that step D by the substrate with film in 100 ~ 120 DEG C,
Anneal 12 ~ 60min under 4.5mTorr, 145mTorr, 290mTorr, 4Torr or 560Torr.
9. preparation method according to claim 1, it is characterised in that substrate described in process B, C, D is transparent conductive film.
10. preparation method according to claim 1, it is characterised in that substrate described in process B, C, D is ITO electro-conductive glass, FTO
Electro-conductive glass or simple glass.
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| CN106119971B (en) * | 2016-07-06 | 2018-06-15 | 福州大学 | A kind of preparation and its application of organic and inorganic perovskite spike crystal |
| 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 |
| 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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