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In this work, the 1,4-diaminobutane (BDA) based DJ perovskites ((BDA)MA4Pb5I16) fabricated by a fast blade-coating method were investigated. Particular attention has been paid to the impacts of HTLs wettability on the bottom morphologies of the blade-coated DJ perovskite films. The employed HTLs include super hydrophilic NiOx, ordinary hydrophilic poly-TPD (poly[N,N′-bis(4-butylphenyl)-N,N′-bisphenylbenzidine]), and PTAA (poly[bis(4-phenyl) (2,4,6-trimethylphenyl)amine]). We proved that the substrate wettability is closely bound up with the yield of pinholes and buried voids in the blade-coated (BDA)MA4Pb5I16 films. Consequently, the (BDA)MA4Pb5I16 PSCs fabricated on super hydrophilic NiOx exhibit largely suppressed bottom voids/pinholes, leading to a champion PCE of 16.26%.
Inspired by our previous study, the DJ type (BDA)MAn-1PbnI3n+1 perovskite films were fabricated by the blade-coating method with the assistance of NH4Cl additive, hot-air flow, and heated substrate (Fig. S1, supplementary material), all of which help to promote the downward growth of 2D perovskites for the out-of-plane orientation.19,2019. J. Wang, S. Luo, Y. Lin, Y. Chen, Y. Deng, Z. Li, K. Meng, G. Chen, T. Huang, S. Xiao, H. Huang, C. Zhou, L. Ding, J. He, J. Huang, and Y. Yuan, Nat. Commun. 11(1), 582–590 (2020). https://doi.org/10.1038/s41467-019-13856-120. J. Ding, Q. Han, Q. Ge, D. Xue, J. Ma, B. Zhao, Y. Chen, J. Liu, D. B. Mitzi, and J. Hu, Joule 3(2), 402–416 (2019). https://doi.org/10.1016/j.joule.2018.10.025 First, it should be mentioned that pristine poly-TPD and PTAA substrates are too hydrophobic to blade-coating fully covered (BDA)MA4Pb5I16 films (Fig. S2). After PFN-Br (poly[9,9-bis(3′-(N,N-dimethyl)-N-ethylammoinium-propyl-2,7-fluorene)-alt-2,7–(9,9-dioctylfluorene)]dibromide) modification,2121. J. Lee, H. Kang, G. Kim, H. Back, J. Kim, S. Hong, B. Park, E. Lee, and K. Lee, Adv. Mater. 29(22), 1606363 (2017). https://doi.org/10.1002/adma.201606363 the improved wettability of these two HTLs confirmed by their decreased contact angles enabled the fabrication of DJ perovskite films with full coverage [Fig. 1(a)]. Therefore, all the poly-TPD and PTAA samples discussed below referred to PFN-Br treated ones, if not specified.(BDA)MA4Pb5I16 films blade-coated on NiOx substrates with high wettability exhibit reduced surface roughness. Based on atomic force microscopy (AFM) topography images, the perovskite films blade-coated on poly-TPD and PTAA showed bigger grain sizes but higher surface roughness of root mean square (RMS) = 30.16 and 23.41 nm (Fig. S3), respectively. On the contrary, perovskite films with smoother surfaces (RMS = 19.34 nm) were obtained on NiOx substrates.
More importantly, the super hydrophilic NiOx substrates lead to (BDA)MA4Pb5I16 films with reduced bottom voids. From the cross section scanning electron microscopy (SEM) images [Fig. 1(b)], the films on poly-TPD and PTAA suffered from rough perovskite/HTL interfaces with obvious voids embedded. In our previous study, with super hydrophilic PEDOT:PSS (poly(3,4-ethylenedioxythiophene):poly(styrenesulfonate)) as substrates, self-generated MA (methylamine) gas was used to in situ heal the nanoscale voids at the bottom of RP type 2D perovskite films.2222. J. Wang, S. Luo, X. Tang, S. Xiao, Z. Chen, S. Pang, L. Zhang, Y. Lin, J. He, and Y. Yuan, ACS Energy Lett. 6(10), 3634–3642 (2021). https://doi.org/10.1021/acsenergylett.1c01771 A similar strategy has also been employed in this study by replacing BDAI2 raw materials with BDA and MAI to generate MA gas. However, the bottom voids cannot be completely suppressed when the PEDOT:PSS is changed to poly-TPD and PTAA. On the contrary, compact, void-free perovskite films were obtained on super hydrophilic NiOx substrates, which offers us this opportunity to further explore the role of substrates on the formation of bottom interface contacts. It should be noted that the 3D perovskite (MAPbI3) films prepared by the same method can form compact bottom contact on ordinary hydrophilic PTAA substrates (Fig. S4). This difference might be related to the introduction of bulky organic cations in 2D perovskites, which changes the surface tension and viscosity of the liquid film.To gain insights into the mechanism of suppressed bottom voids on super hydrophilic NiOx substrates, we monitored the drying process of perovskite precursor solution droplet [∼0.25 μl, 0.2 M (BDA)MA4Pb5I16 in DMF] on these three kinds of HTLs [Fig. 1(c)]. As the solvent evaporates, the contact line of the droplet boundary retracts significantly on poly-TPD (or PTAA) substrate, while it remains nearly stationary on NiOx substrate. By calculating the coverage change against time, the free dewetting speed of the precursor solution on different substrates can be quantitatively compared [Figs. 1(d) and S5]. The coverage of droplets on poly-TPD and PTAA substrates drops to 10% and 50% of their initial values within three minutes, respectively. By contrast, the droplet spreads remarkably on the NiOx substrate due to its super wettability (θ3 solution was observed even on ordinary hydrophilic PTAA (Fig. S6), which explains the void-free bottom contact formed in the corresponding film (Fig. S4).The liquid film dewetting tendency during blade-coating is closely related to its contact angle on substrate. As illustrated in Fig. 1(e), the contact angle is determined by the following Young's equation: where ΔγS is the interfacial energy difference between solid/gas interface (γSG) and solid/liquid interface (γSL) and γLG is the interfacial energy of liquid/gas interface.2323. J. Yong, F. Chen, Q. Yang, J. Huo, and X. Hou, Chem. Soc. Rev. 46(14), 4168–4217 (2017). https://doi.org/10.1039/C6CS00751A According to study of Edwards et al.,2424. A. M. J. Edwards, R. Ledesma-Aguliar, M. I. Newton, C. V. Brown, and G. McHale, Sci. Adv. 2(9), 1600183 (2016). https://doi.org/10.1126/sciadv.1600183 the dewetting speed of liquid films driven by surface tension is sensitive to the equilibrium contact angle by where the surface tension (γLG) and the viscosity (η) of precursor solution do not change with substrates. However, the dewetting speed υ (∝θ3) increases by two orders of magnitude when changing the substrate from NiOx to poly-TPD or PTAA, which potentially explains the significantly different density of voids [Fig. 1(b)] when perovskite films are blade coated on different hydrophilic substrates.Based on the relationship between dewetting speed and density of voids observed above, we propose a model for further explanation, which focused on the later stage of the solution drying. As previously reported, 2D perovskites crystallize from the top of solution, preferentially forming a porous crust on the upper surface of the residual solution.2525. Y. Lin, Y. Fang, J. Zhao, Y. Shao, S. J. Stuard, M. M. Nahid, H. Ade, Q. Wang, J. E. Shield, N. Zhou, A. M. Moran, and J. Huang, Nat. Commun. 10(1), 1008 (2019). https://doi.org/10.1038/s41467-019-08958-9 As the solvent volatilizes, the gradually decreased solution volume can be compensated by the descent of the crust. As illustrated in Fig. 2(a), when the rough growth front of the perovskite crust partially touches the substrate, the decreased solution volume cannot be compensated by the descent of the perovskite crust. From this moment on, the location of the liquid film is determined by the competition between the capillary forces on its top side (with perovskite crust) and bottom side (with substrate). Specifically, in the case of poly-TPD or PTAA as substrate, the wettability of solution with the top porous perovskite crust (θtop∼0°) and the bottom substrate (θbott>30°) is quite different. Therefore, a surface-tension-induced capillary pressure difference (ΔPc) formed between the top and bottom sides.2626. B. Zhao, J. S. Moore, and D. J. Beebe, Science 291(5506), 1023–1026 (2001). https://doi.org/10.1126/science.291.5506.1023 As the solution volume persistently decreases, ΔPc draws the residual solution to shift upward and cause depressurization at the bottom of solution. This process needs to be assisted by forming bubbles at the bottom of solution because the liquid is non-expandable, so the capability for bubbles to grow on the substrate/solution interface is a key issue to influence the yield of bottom voids.To visualize the fundamental difference between ordinary hydrophilic substrate and super hydrophilic substrate in the formation of interfacial bubbles, poly-TPD and NiOx coated substrates are intentionally soaked into DMF solution (T = 50 °C) to compare the bubble formation rate. Air-evacuation was applied here to mimic the solution depressurization induced by the capillary effect. When the pressure was reduced to ∼0.01 MPa, massive bubbles were formed on the poly-TPD substrate [Fig. 2(b)], but nearly no bubbles were formed on the NiOx surface. This observation supports the idea that super hydrophilic substrates are more capable of repelling bubbles than ordinary hydrophilic substrates, which is consistent with the conclusion of Yong et al.2727. J. Yong, F. Chen, Y. Fang, J. Huo, Q. Yang, J. Zhang, H. Bian, and X. Hou, ACS Appl. Mater. Interfaces 9(45), 39863–39871 (2017). https://doi.org/10.1021/acsami.7b14819The dynamical formation and dissolution of bubble are analogous to the heterogeneous nucleation of solute on a substrate, which is highly related to its contact angle with the substrate.2828. K. J. Vachaparambil and K. E. Einarsrud, J. Electrochem. Soc. 165(10), E504–E512 (2018). https://doi.org/10.1149/2.1031810jes An occasional bubble nucleus can be formed by thermal fluctuations.2929. G. Nagashima, E. V. Levine, D. P. Hoogerheide, M. M. Burns, and J. A. Golovchenko, Phys. Rev. Lett. 113(2), 024506 (2014). https://doi.org/10.1103/PhysRevLett.113.024506 Once its radius exceeds the critical radius r*, the bubble nucleus will grow continuously to lower the Gibbs free energy, and vice versa [Fig. 2(c)]. On the poly-TPD or PTAA substrate, the liquid film tends to retract once a bubble nucleus is formed, which, hence, promotes the growth of bubble and eventually the formation of buried voids [Fig. 2(d)]. This kind of structural defect is too large to be healed during the thermal annealing process by crystal ripening (Fig. S7). In contrast, the occasional bubble nucleus tends to be compressed on NiOx substrate due to the strong liquid spreading effect, which leads to the reduced voids by 1–2 orders of magnitude.Pinhole is another kind of common structural defect that is widely hidden in large-area perovskite films. It is also important to clarify that the formation mechanism of pinholes is not necessarily the same as the bottom voids. According to a typical dewetting theory,3030. A. Sharma and E. Ruckenstein, J. Colloid Interface Sci. 133(2), 358–368 (1989). https://doi.org/10.1016/S0021-9797(89)80044-X the dynamic deformation of liquid film surface induced by external fluctuations can cause the formation of pinholes. The retracting tendency of the contact line would stabilize those occasionally generated pinholes [Fig. 3(a)]. Conversely, the spreading tendency of the contact line would eliminate occasional pinholes [Fig. 3(b)]. Sharma et al. propose a critical thickness (h*) to describe the capability of forming pinholes on substrates,3030. A. Sharma and E. Ruckenstein, J. Colloid Interface Sci. 133(2), 358–368 (1989). https://doi.org/10.1016/S0021-9797(89)80044-X Once the initial height of the liquid film is less than h*, the probability of forming stable pinholes increases dramatically. From the equation above, the h* is quite sensitive to the θ, e.g., the h* decreased by 7 times when replacing PTAA (or poly-TPD) with NiOx. For 2D perovskite films with unchanged thickness, the decrease in h* in turn offers a lower pinhole density. To further prove the relationship between substrate wettability and pinhole density, the film thicknesses were intentionally reduced from 400 to 150 nm [Figs. 3(c)–3(f)]. The pinhole densities of films on poly-TPD and PTAA are one order of magnitude higher than that of NiOx-based films at different thicknesses, which agree well with our hypothesis.In addition, the adhesion strength of the perovskite/HTL interface was further characterized by mechanically peeling the perovskite film off the substrate. In our study, almost the whole films on poly-TPD and PTAA could be readily peeled off, but the film on NiOx substrate could not be peeled off regardless of the substrate temperature [Figs. 3(g) and S8)]. The strong adhesion between (BDA)MA4Pb5I16 and NiOx might be ascribed to the suppressed bottom voids and the formation of hydrogen bonds between the hydroxyl groups on NiOx surface and the amine groups on BDA molecules or the I− on [PbI6]4− octahedron network.31,3231. J. R. Manders, S. W. Tsang, M. J. Hartel, T. H. Lai, S. Chen, C. M. Amb, J. R. Reynolds, and F. So, Adv. Funct. Mater. 23(23), 2993–3001 (2013). https://doi.org/10.1002/adfm.20120226932. J. You, L. Meng, T. B. Song, T. F. Guo, Y. M. Yang, W. H. Chang, Z. Hong, H. Chen, H. Zhou, Q. Chen, Y. Liu, N. De Marco, and Y. Yang, Nat. Nanotechnol. 11(1), 75–81 (2016). https://doi.org/10.1038/nnano.2015.230To compare the photovoltaic performance of PSCs based on these three HTLs, devices with the planar structure of ITO/HTL/perovskite/PC61BM/BCP/Cu were fabricated [Fig. 4(a)]. The champion PCEs of blade-coated (⟨n⟩ = 5) DJ PSCs are 9.83%, 10.95%, and 16.26% on poly-TPD, PTAA, and NiOx, respectively [Fig. 4(b) and S9, Table S1]. The statistical analysis further confirms the superior reproducibility and the substantial improvements in all photovoltaic merits of NiOx-based solar cells [Fig. 4(c)]. The PCE improvement reported here is quite promising because blade-coated DJ perovskite solar cells with PCE over 16% are still sparse to date (Table S2).3333. Y. Chen, J. Hu, Z. Xu, Z. Jiang, S. Chen, B. Xu, X. X. Liu, K. Forberich, C. J. Brabec, Y. Mai, and F. Guo, Adv. Funct. Mater. 32(19), 2112146 (2022). https://doi.org/10.1002/adfm.202112146 The NiOx-based cells show an overall improved EQE in the whole range of 300–750 nm compared to poly-TPD- and PTAA-based cells [Fig. 4(d)], which suggests a more effective charge collection due to the reduced interfacial voids and enhanced interfacial binding in NiOx-based cells. In addition, the dark current densities of NiOx-based cells (at −0.2 V) are nearly one order of magnitude lower than that of poly-TPD- and PTAA-based cells [Fig. 4(e)], which is in good agreement with the reduced pinholes observed in perovskite films on NiOx substrates.All the related devices have been studied by transient photovoltage (TPV), transient photocurrent (TPC), and thermal admittance spectroscopy (TAS) techniques (Fig. S10). As shown in Fig. 5(a), the carrier recombination lifetime obtained from TPV measurement increased from 0.46 ± 0.04 μs for the poly-TPD (and 0.52 ± 0.03 μs for PTAA) based devices to 1.16 ± 0.02 μs for NiOx based devices, which was attributed to the reduced interfacial voids that have been shown in Fig. 1(b). The faster TPC decay in NiOx-based device than that in poly-TPD- and PTAA-based devices indicated a significantly faster charge-extraction [Fig. 5(b)].3434. Z. Xiao, Q. Dong, C. Bi, Y. Shao, Y. Yuan, and J. Huang, Adv. Mater. 26(37), 6503 (2014). https://doi.org/10.1002/adma.201401685 The trap density of states (tDOS) of the DJ perovskite films has been measured by TAS [Fig. 5(c)]. The NiOx-based device also shows lower tDOS in the trap depth region of 0.35–0.45 eV, as compared to those of the two other samples. Furthermore, the faster charge transport in NiOx-based cells can also be confirmed by the light intensity (P)-dependent J–V results. Under weak light conditions, the FF of poly-TPD- and PTAA-based cells gradually decreases with increased light intensity, which strongly suggests that their low FF under AM 1.5 G condition is limited by their inefficient charge extraction at the HTL/perovskite interfaces [Fig. 5(d)]. The FF of NiOx-based cells (∼74%) is stable in a wide light intensity range of 1–100 mW cm−2, demonstrating the more efficient charge extraction.It is worth pointing out that the NiOx-based cells show superior UV stability than those based on the most popular PTAA HTL.35,3635. Y. Deng, S. Xu, S. Chen, X. Xiao, J. Zhao, and J. Huang, Nat. Energy 6(6), 633–641 (2021). https://doi.org/10.1038/s41560-021-00831-836. X. Zheng, Y. Hou, C. Bao, J. Yin, F. Yuan, Z. Huang, K. Song, J. Liu, J. Troughton, N. Gasparini, C. Zhou, Y. Lin, D. J. Xue, B. Chen, A. K. Johnston, N. Wei, M. N. Hedhili, M. Wei, A. Y. Alsalloum, P. Maity, B. Turedi, D. Baran, T. D. Anthopoulos, Y. Han, Z. H. Lu, O. F. Mohammed, F. Gao, E. H. Sargent, and O. M. Bakr, Nat. Energy 5(2), 131–140 (2020). https://doi.org/10.1038/s41560-019-0538-4 When the cells are illuminated by UV light with a wavelength of 395 nm and an intensity of 50 mW cm−2, the PTAA-based cell undergoes a sharp efficiency decline to 10% of its initial PCE after 50 kWh m−2 irradiation [Fig. 5(e)]. In contrast, the NiOx-based cell maintains 80% of its initial PCE. This improvement might be not only directly benefited from the improved bottom interface contact but more likely related to the intrinsically better UV stability of NiOx than PTAA materials.At last, PSCs with active areas of 1.05 cm2 are also fabricated to evaluate film quality over a larger scale. As shown in Fig. 5(f), the best-performing large-area device exhibited VOC, JSC, and FF values of 1.129 V, 18.52 mA cm−2, and 55.8%, respectively, yielding a high PCE of 11.65%. The superior photovoltaic performance of NiOx-based devices than that of poly-TPD- and PTAA-based cells further demonstrated the importance of suppressing the pinholes and bottom voids in large-area PSCs (Fig. S11 and Table S3).In summary, BDA-based DJ-type perovskite solar cells with good reproducibility and best PCE of 16.26% have been achieved by the blade-coating method. We demonstrate that NiOx substrate with super hydrophilicity and strong bubble repellency is essentially better than hydrophilic poly-TPD and PTAA substrates in the aspect of suppressing pinholes and buried voids. The strong spreading tendency of perovskite precursor solution on NiOx thermal dynamically suppresses the nucleation and growth of bubbles during the drying process. The strong adhesion between the (BDA)MA4Pb5I16 film and the NiOx promotes the interfacial charge extraction, leading to improved photocurrent and fill factor in the resulting PSCs. The (BDA)MA4Pb5I16 PSCs on NiOx have better UV stability than those on PTAA substrate, which can survive UV light irradiation with an energy dosage of 50 kWh m−2. This work pays insights into the formation mechanisms of pinholes and buried voids in perovskite thin films and provides a simple strategy to fabricate large-area pinhole- and void-free perovskite films with super hydrophilic substrates.
See the supplementary material for the device preparation and characterization methods, the schematic of blade coating (Fig. S1); photographs of blade coated 2D perovskite films on pristine HTLs (Fig. S2); atomic force microscope (AFM) and top-view SEM of the perovskite films (Fig. S3); section SEM of 3D and 2D perovskite film on PTAA (Fig. S4); contact angle evolution of precursor solution droplets on the three HTLs (Fig. S5); evolution of 2D and 3D perovskite droplets on PTAA (Fig. S6); the bottom SEM images of perovskite films before and after annealing (Fig. S7); mechanically peeling the films off from HTLs (Fig. S8); the stabilized power output of the champion device and J–V curves (Fig. S9); the photovoltage decay and photocurrent decay (Fig. S10); J–V curves of large-area PSCs (Fig. S11); the photovoltaic parameters of the champion device based on the three HTLs (Table S1); the photovoltaic parameters of 2D PSCs based on straight chain diamine molecule (Table S2); and photovoltaic parameters of large-area PSC (Table S3).The authors acknowledge financial support from the National Natural Science Foundation of China under Grant Nos. 62104261, 52273202, 51673218, 61874141, and 62004066. Y.L. acknowledges support from the program of Hundreds of Talents of Hunan Province. Y.Y. acknowledges support from the Innovation-Driven Project of Central South University (No. 2020CX006) and the Hunan Provincial Science & Technology Department (No. 2017XK2030). L.Z. acknowledges support from the Natural Science Foundation of Hunan Province (No. 2021JJ20077). Y.L. acknowledges support from the Changsha Municipal Natural Science Foundation (No. KQ2007027). X.R. acknowledges support from the Postgraduate Independent Exploration and Innovation Project of Central South University (No. 2020ZZTS366) and the Postgraduate Innovation Project of Hunan Province (No. CX20200151). J.W. acknowledges support from the Natural Science Foundation of Hunan Province (No. 2021JJ30303) and the Youth Fund of Education Department of Hunan Province (No. 19B242).
Conflict of Interest
The authors have no conflicts to disclose.
Author Contributions
Wen Deng: Data curation (lead); Formal analysis (lead); Investigation (lead); Methodology (lead); Writing – original draft (lead); Writing – review & editing (equal). Lin Zhang: Investigation (equal); Writing – review & editing (equal). Bin Yang: Writing – review & editing (equal). Jun He: Writing – review & editing (supporting). Yongbo Yuan: Conceptualization (equal); Formal analysis (equal); Investigation (equal); Supervision (equal); Writing – review & editing (equal). Yun Lin: Conceptualization (equal); Data curation (equal); Formal analysis (equal); Funding acquisition (equal); Investigation (equal); Methodology (equal); Supervision (equal); Writing – review & editing (equal). Fang Wan: Investigation (supporting). Xinxin Peng: Investigation (supporting). Xiaoxue Ren: Methodology (supporting). Jifei Wang: Formal analysis (supporting). Nan Wu: Methodology (supporting). Weiran Qin: Methodology (supporting). Xiaohui Gao: Methodology (supporting). Si Xiao: Investigation (equal).
The data that support the findings of this study are available within the article and its supplementary material.REFERENCES
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