CN111129314A - Preparation method of perovskite electron transport layer - Google Patents
Preparation method of perovskite electron transport layer Download PDFInfo
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Abstract
The invention provides a preparation method of a perovskite electron transport layer, and belongs to the technical field of perovskite solar cells. The method takes an aqueous solution of titanium tetrachloride as a source solution, takes an alcoholic solution of niobium pentachloride as a doping solution, and controls the substitution ratio of niobium element of the final film-forming material by changing the solute molar ratio of the source solution and the doping solution, thereby continuously adjusting the energy level energy band position of the material; the morphology of the final film-forming material is controlled by adjusting the proportion of solvent water in the source solution to alcohol in the doping solution, so that the one-time preparation of the compact layer and the mesoporous layer is realized, and the construction of the lag-free perovskite battery is realized; and the whole preparation process is finished under one hundred ℃, the requirement on the substrate is not high, and the energy dissipation is low.
Description
Technical Field
The invention belongs to the technical field of perovskite solar cells, and particularly relates to a preparation method of a perovskite electron transport layer doped with titanium oxide.
Background
As one of emerging photovoltaic technologies, perovskite solar cells are known as the fastest-developing photovoltaic technology, and the photovoltaic conversion efficiency of the perovskite solar cells can reach more than 25% as of 2019. Such photovoltaic cell structures often employ a sandwich-type, p-i-n or n-i-p structure, i.e., an i-type perovskite light absorption layer is sandwiched by an n-type semiconductor electron transport layer and a p-type semiconductor hole transport layer to achieve carrier extraction, and thus the energy conversion efficiency of the perovskite photovoltaic cell is not only determined by the perovskite light absorption material but also is closely related to the mass of the carrier transport layer.
Titanium oxide has been used as an electron transport layer of a perovskite battery for a long time, and the compounding of a titanium oxide dense layer and a mesoporous layer is reported in the literature, so that the photovoltaic conversion efficiency of more than 22 percent can be obtained[1]However, the titanium oxide material also has disadvantages, firstly, the titanium oxide material has poor conductivity, and only needs a very thin layer of thickness as an electron transport layer, but the preparation is easy to be uneven by adopting processes such as sputtering or spin coating, and the like, and the preparation time is too long (about 10nm needs several hours) by adopting the atomic layer deposition technology, so the preparation method is not suitable for the requirement of large-area preparation; in addition, the low conductivity and high defect of titanium oxide make the surface easy to accumulate charges, so that the device presents low filling factor and high hysteresis (J-V tests have different scanning direction curves which are not coincident). In order to solve these problems, it is necessary to select a suitable method for preparing titanium oxide and doping modification.
There are many methods for doping modification of titanium oxide electron transport layers, and the elements involved span almost all the metal elements on the periodic table, and the use of some non-metal elements and their corresponding simple substances and compounds has also been reported (F, C, etc.). For element doping, most important is the matching of the radius, and the similar ionic radius can not only improve the solid solubility of substitutional doping, but also reduce the stress effect in the crystal during doping and reduce the generation of defects such as dislocation and the like. In the titanium oxide crystal, titanium metal is in a tetravalent state, and a pentavalent metal having a similar ionic radius is the most preferable. Niobium metal (Nb) has an ionic radius (Nb) similar to that of titanium5+About 70pm, Ti4+About 68pm) and its pentavalent form is stable, is widely selected as a doping of titanium oxide electron transport materialsAnd (3) preparing. Some working options are to combine Nb: TiO 22Growing nanostructures onto a substrate[2]However, the nanoparticles prepared in this way can only serve as mesoporous layers to provide a support structure for perovskite materials, and in order to form a complete battery, other processes are also needed to prepare a titanium oxide dense layer to prevent direct contact of perovskite-substrate; similarly, Nb-TiO prepared by coating-annealing process2The film can only be used as a compact layer, and the mesoporous structure of the film needs other steps for secondary preparation[3](ii) a Of course, there are also research options to directly discard the mesoporous layer, using only one layer of Nb-TiO2The thin film constructs the plane structure battery, but the devices constructed by the operation all show larger hysteresis[4]. In addition, crystallization of titanium oxide often requires high temperatures of several hundred degrees, which greatly increases the cost of device fabrication and limits the range of choices for device substrates, such as PET substrates for flexible devices that cannot withstand high temperatures greater than 100 ℃. Many efforts have been made to achieve low temperature crystallization of titanium oxide, such as replacing the Ti source to achieve a different reaction path, or by uv treatment to crystallize the sample[5]But none can solve the performance degradation of the lost mesoporous layer.
[1]Yang,W.S.；Park,B.W.；Jung,E.H.；Jeon,N.J.；Kim,Y.C.；Lee,D.U.；Shin,S.S.；Seo,J.；Kim,E.K.；Noh,J.H.；et al.Iodide Management in Formamidinium-Lead-Hali de-Based Perovskite Layers for Efficient Solar Cells.Science 2017,356,1376–1379.
[2]Yang,M.；Guo,R.；Kadel,K.；Liu,Y.；O’Shea,K.；Bone,R.；Wang,X.；He,J.；Li,W.Improved Charge Transport of Nb-Doped TiO 2Nanorods in Methylammonium LeadIodide Bromide Perovskite Solar Cells.J.Mater.Chem.A 2014,2,19616–19622.
[3]Yin,X.；Guo,Y.；Xue,Z.；Xu,P.；He,M.；Liu,B.Performance Enhancement ofPerov skite-Sensitized Mesoscopic Solar Cells Using Nb-Doped TiO2 CompactLayer.Nano Res.2015,8,1997–2003.
[4]Yin,G.；Ma,J.；Jiang,H.；Li,J.；Yang,D.；Gao,F.；Zeng,J.；Liu,Z.；Liu,S.F.Enhancing Efficiency and Stability of Perovskite Solar Cells through Nb-Doping of TiO2 at Low Temperature.ACS Appl.Mater.Interfaces 2017,9,10752–10758.
[5]Jeong,I.；Jung,H.；Park,M.；Park,J.S.；Son,H.J.；Joo,J.；Lee,J.；Ko,M.J.ATailored TiO2 Electron Selective Layer for High-Performance FlexiblePerovskite Solar Cells via Low Temperature UV Process.Nano Energy 2016,28,380–389.
Disclosure of Invention
In view of the problems in the background art, the present invention is directed to a perovskite electron transport layer and a method for preparing the same. The method takes an aqueous solution of titanium tetrachloride as a source solution, takes an alcoholic solution of niobium pentachloride as a doping solution, and controls the substitution ratio of niobium element of the final film-forming material by changing the solute molar ratio of the source solution and the doping solution, thereby continuously adjusting the energy level energy band position of the material; the morphology of the final film-forming material is controlled by adjusting the proportion of solvent water in the source solution to alcohol in the doping solution, so that the one-time preparation of the compact layer and the mesoporous layer is realized, and the construction of the lag-free perovskite battery is realized.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a perovskite electron transport layer comprises the following steps:
step 1, freezing ultrapure water to enable the ultrapure water to be in an ice-water mixed state, stirring at 0-4 ℃, dropwise adding liquid titanium tetrachloride, stirring at room temperature until the ice-water mixture is just dissolved after dropwise adding is finished to obtain a source solution, and storing at 0-4 ℃ after the solution is wholly light yellow, clear and transparent;
and 6, taking out the substrate after the reaction is finished, sequentially soaking the substrate in water-alcohol-water for cleaning, and removing residual reaction liquid to obtain the perovskite electron transport layer.
Further, the concentration of the titanium tetrachloride in the source solution in the step 1 is 0.01-0.5 mol/L.
Further, the alcohol in the step 2 is methanol or absolute ethanol, the alcohol can dissolve the niobium pentachloride without hydrolysis, has a lower boiling point, preferentially evaporates compared with water in a water bath, and the concentration of the niobium pentachloride in the doping liquid is 0.01-0.1 mol/L.
Further, the substrate in step 3 is a transparent conductive oxide substrate, specifically fluorine-doped tin oxide (FTO), antimony-doped tin oxide (ATO), or the like.
Further, in step 5, the air-impermeable film is a PET film, a polyimide film or the like.
Further, the heating reaction temperature in the step 5 is 60-80 ℃, and the reaction time is 30 min-3 h.
Further, the alcohol used in step 6 and the alcohol used in step 2 are the same alcohol.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the preparation method, the perovskite electron transport layer of the niobium doped titanium oxide nanoneedle is generated by co-hydrolyzing the aqueous solution of titanium tetrachloride and the alcoholic solution of niobium pentachloride, the final film forming appearance is changed by adjusting the ratio of the solvent in the source solution and the doping solution, the structure preparation of the compact layer and the mesoporous layer can be simultaneously realized in one continuous reaction, the whole preparation process is finished at a temperature below one hundred ℃, the requirement on the substrate is low, and the energy dissipation is low.
2. According to the invention, the doping amount of niobium in the perovskite electron transport layer film can be changed by the ratio of the molar amount of the Nb element in the total element molar amount of Nb and Ti in the preparation method, so that the energy level energy band is continuously adjusted, the energy band structure of the film is more biased to the vacuum energy level when the doping amount of the Nb element is higher, the change is continuously controllable, and the selection range of the perovskite absorption layer matched with the film is wider.
3. The reaction mechanism of the invention is thermal hydrolysis reaction under normal temperature and pressure, large-area preparation can be completed only by a large enough reaction vessel and a large enough reaction solution, professional equipment such as a spin coating instrument, a vacuum pump and the like is not needed, and the invention is suitable for industrial production.
Drawings
FIG. 1 is an SEM topography of perovskite electron transport layers prepared by reaction with different Nb doping amounts;
wherein a is 0% of the molar amount of the Nb element in comparative example 1, b is 2% of Nb, c is 4% of Nb, d is 6% of Nb, e is 8% of Nb, and f is 10% of Nb.
FIG. 2 is an SEM topography of perovskite electron transport layers prepared with different absolute ethanol-water solvent ratios;
wherein a is the topography of the electron transport layer prepared in example 3; b is the topography of the electron transport layer prepared in example 4.
FIG. 3 is an X-ray photoelectron spectroscopy (XPS) plot of perovskite electron transport layers prepared by different Nb doping reactions;
wherein a is 0% Nb, b is 2% Nb, c is 4% Nb, d is 6% Nb, e is 8% Nb, and f is 10% Nb in comparative example 1.
FIG. 4 is an energy level band diagram of perovskite electron transport layers prepared by different Nb doping reactions.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following embodiments and accompanying drawings.
The invention realizes the continuous growth of two morphologies of the same material in the one-step growth process by volatilization of the low-boiling-point alcohol, and can realize the continuous regulation and control of the energy level energy band position of the electron transport layer film by changing the actual doping amount of the niobium element in the electron transport layer film.
Example 1
A preparation method of a perovskite electron transport layer comprises the following steps:
step 1, freezing 400mL of ultrapure water to enable the ultrapure water to be in an ice-water mixed state, stirring at 0 ℃, dropwise adding 4.4mL of liquid titanium tetrachloride, stirring at room temperature until the ice-water mixture is just dissolved after dropwise adding is finished to obtain a source solution, wherein the whole solution is light yellow, clear and transparent, and then storing at 0 ℃;
and 6, taking out the substrate after the reaction is finished, sequentially soaking the substrate in water, absolute ethyl alcohol and water for cleaning, and removing residual reaction liquid to obtain the perovskite electron transport layer.
Example 2
The perovskite electron transport layer was prepared as in example 1, and only the volumes of the dopant solution and the source solution in step 4 were adjusted so that the molar amount of Nb element in the mixed solution was 4%, 6%, 8%, and 10% of the total molar amount of Nb and Ti, and the perovskite electron transport layer was prepared without changing the other steps.
Example 3
Preparing a perovskite electron transport layer according to the embodiment 1, and adjusting the volume of the solvent in the step 2 to be 10ml, namely, the concentration of the doping liquid is improved by 10 times; in the step 4, the volume of the doping liquid is adjusted to be 30 μ L, the total doping concentration of Nb is 10%, the molar weight of Nb is 10% of the total molar weight of Nb and Ti, and the volume ratio of absolute ethyl alcohol to water in the solvent of the mixed solution is 1%.
Example 4
The perovskite electron transport layer was prepared as in example 1, adjusting the niobium pentachloride in step 2 to 0g, i.e. using only absolute ethanol as the doping liquid, the remaining steps being unchanged.
Comparative example 1
Step 1, freezing 400mL of ultrapure water to enable the ultrapure water to be in an ice-water mixed state, stirring at 0 ℃, dropwise adding 4.4mL of liquid titanium tetrachloride, stirring at room temperature until the ice-water mixture is just dissolved after dropwise adding is finished to obtain a source solution, wherein the whole solution is light yellow, clear and transparent, and then storing at 0 ℃;
2, ultrasonically cleaning a 1 cm-by-1 cm FTO substrate for 20min by using acetone, ethanol and water in sequence, and then treating the FTO substrate in an ultraviolet-ozone environment for 20min to make the surface hydrophilic;
and 5, taking out the substrate after the reaction is finished, sequentially soaking the substrate in water, absolute ethyl alcohol and water for cleaning, and removing residual reaction liquid to obtain the perovskite electron transport layer.
The SEM topography of the perovskite electron transport layer prepared in this comparative example is shown in fig. 1 (a).
Fig. 1 is an SEM topography of a perovskite electron transport layer prepared by reaction with different Nb doping amounts of the present invention, that is, an SEM topography of a thin film after reaction under different ratios of the molar amount of Nb element in a mixed solution to the molar amount of total elements Nb and Ti, as can be seen from the figure, except for the figure (a), the molar amounts of other Nb elements account for the ratio, and the figures (b) to (f) are nanoneedles completely coated on FTO grains, which illustrates that the niobium-titanium solute ratio does not control the growth morphology; the reason why the compact shape of the nano-particles is shown in the graph (a) is that the shape of the nano-needle cannot be prepared due to the loss of alcohol-water mixed reaction under the condition that all solvents are water, namely, the co-hydrolysis of water and alcohol solution required for the structure preparation of the compact layer and the mesoporous layer is simultaneously realized in one continuous reaction.
FIG. 2 is an SEM image of perovskite electron transport layers prepared by different ratios of absolute ethanol to water solvent, wherein FIG. 2a is an SEM image of a thin film after reaction of mixed liquid in example 3 of the present invention, the molar amount of Nb is 10% of the total molar amount of Nb and Ti, but the ratio of absolute ethanol to water solvent is only 1%, and in combination with (f) in FIG. 1, it can be seen that as the ratio of absolute ethanol is reduced, the needle-like morphology in the final thin film is reduced; fig. 2b is an SEM morphology of the thin film after the mixed solution reaction of example 4, that is, the thin film is obtained by adding only 2% by volume of absolute ethanol without adding any Nb solute, and it can be found that the nanoneedle-like morphology is realized without depending on Nb element, and only by adjusting the proportion of absolute ethanol, it is further demonstrated that the morphology of the dense-mesoporous pores in the invention is independently controlled by the ratio of alcohol and water solvent in the mixed solution, that is, the ratio of alcohol in the solvent is the key to control the morphology.
Fig. 3 is an X-ray photoelectron spectroscopy (XPS) graph of perovskite electron transport layers prepared by different Nb to Ti solute ratios of the present invention, and from the graph (a) to the graph (f), the molar ratio of Nb element in the total element molar amount of Nb and Ti can be seen, it can be seen that the peak intensity belonging to Nb in the film is sequentially increased, and the Nb doping content in the actually prepared electron transport layer is also sequentially increased, i.e. the Nb element ratio of the final film formation and the solute ratio in the mixed solution (i.e. the molar ratio of Nb element) show positive correlation, which proves that the continuous change of the element in the final film formation transport layer film can be realized by adjusting the ratio of Nb in the precursor.
FIG. 4 is a diagram showing the energy band diagram of the thin film after the mixed solution of Nb and Ti in the present invention reacts with the solute ratio, and it can be seen that with TiO2The typical n-type doping trend is that the doping proportion of Nb in the film is increased, the conduction band is gradually moved upwards, and the Fermi level position is gradually close to the conduction band, which shows that the doping of Nb element to Ti can continuously change the energy level energy band position of the film, so that the selection range of the perovskite absorption layer matched with the film is wider.
While the invention has been described with reference to specific embodiments, any feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise; all of the disclosed features, or all of the method or process steps, may be combined in any combination, except mutually exclusive features and/or steps.
Claims (10)
1. A preparation method of a perovskite electron transport layer is characterized by comprising the following steps:
step 1, freezing ultrapure water to enable the ultrapure water to be in an ice-water mixed state, stirring at 0-4 ℃, dropwise adding liquid titanium tetrachloride, stirring at room temperature after dropwise adding until the ice-water mixture is dissolved to obtain a source solution, and then storing at 0-4 ℃;
step 2, adding niobium pentachloride powder into alcohol, and stirring at room temperature until the niobium pentachloride powder is completely dissolved to obtain a doping liquid;
step 3, cleaning the substrate, and then carrying out hydrophilic treatment;
step 4, placing the substrate processed in the step 3 into a reaction container, dripping the doping liquid firstly, and then dripping the source solution until the substrate is completely immersed, wherein n isNb/n(Nb+Ti)≤10％；
Step 5, sealing the reaction container, and then carrying out heating reaction;
and 6, taking out the substrate after the reaction is finished, sequentially soaking the substrate in water-alcohol-water for cleaning, and removing residual reaction liquid to obtain the perovskite electron transport layer.
2. The method for producing the perovskite electron transport layer as claimed in claim 1, wherein the concentration of titanium tetrachloride in the source solution in the step 1 is 0.01 to 0.5 mol/L.
3. The process for preparing a perovskite electron transport layer as claimed in claim 1, wherein the alcohol in step 2 is methanol or absolute ethanol.
4. The method for preparing the perovskite electron transport layer as claimed in claim 1, wherein the concentration of niobium pentachloride in the doping liquid in the step 2 is 0.01-0.1 mol/L.
5. The process for preparing a perovskite electron transport layer as claimed in claim 1, wherein the substrate in step 3 is a transparent conductive oxide substrate.
6. The method of making the perovskite electron transport layer of claim 5, wherein the transparent conductive oxide substrate is fluorine doped tin oxide or antimony doped tin oxide.
7. The process for preparing a perovskite electron transport layer as claimed in claim 1, wherein in step 5 the reactor is sealed with a gas impermeable membrane.
8. The process for preparing a perovskite electron transport layer as claimed in claim 7, wherein the gas impermeable film is a PET film or a polyimide film.
9. The preparation method of the perovskite electron transport layer as claimed in claim 1, wherein the heating reaction temperature in the step 5 is 60-80 ℃ and the reaction time is 30 min-3 h.
10. The process for preparing a perovskite electron transport layer as claimed in claim 1, wherein the alcohol used in step 6 and the alcohol used in step 2 are the same alcohol.
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| US20120125414A1 (en) * | 2010-11-24 | 2012-05-24 | Ricoh Company, Ltd. | Photoelectric converter |
| CN105895807A (en) * | 2016-05-06 | 2016-08-24 | 郑州大学 | Preparation method of TiO2-dopted film |
| CN106025075A (en) * | 2016-06-24 | 2016-10-12 | 华南师范大学 | Method for manufacturing high-performance perovskite solar energy cell in humid air |
| CN106011785A (en) * | 2016-06-07 | 2016-10-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing high-uniformity Nb-doped TiO2 transparent conducting thin film through atomic layer deposition |
| CN108689610A (en) * | 2018-06-26 | 2018-10-23 | 浙江大学 | A kind of titania-doped coated glass of niobium and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120125414A1 (en) * | 2010-11-24 | 2012-05-24 | Ricoh Company, Ltd. | Photoelectric converter |
| CN105895807A (en) * | 2016-05-06 | 2016-08-24 | 郑州大学 | Preparation method of TiO2-dopted film |
| CN106011785A (en) * | 2016-06-07 | 2016-10-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing high-uniformity Nb-doped TiO2 transparent conducting thin film through atomic layer deposition |
| CN106025075A (en) * | 2016-06-24 | 2016-10-12 | 华南师范大学 | Method for manufacturing high-performance perovskite solar energy cell in humid air |
| CN108689610A (en) * | 2018-06-26 | 2018-10-23 | 浙江大学 | A kind of titania-doped coated glass of niobium and preparation method thereof |
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