Properties of a ZnO:B Layer Fabricated by LPCVD and Its Application in Perovskite Solar Cells

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Properties of a ZnO:B Layer Fabricated by LPCVD and Its Application in Perovskite Solar Cells

https://doi.org/10.21203/rs.3.rs-5213960/v1

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A process for finding inexpensive materials for use in perovskite solar cell applications is an interesting task for research aimed at reducing the cost of producing samples.

To address this problem, the application of a metal oxide can be helpful. Metal oxides have always attracted attention due to their combination of conductive and optic properties. Among them, zinc oxide stands out. Zinc oxide films, which are nontoxic and easy to produce, have a suitable band gap and can be recommended as promising materials in optoelectronics.

In this work, the results of the research of a ZnO film doped with boron (ZnO:B) on glass substrates were obtained via the LPCVD (low-pressure chemical vapor deposition) method. The surface, electrical, structural, and optical properties of the ZnO:B layer were studied. The application of a ZnO:B layer in planar perovskite solar cells was demonstrated. The fabricated test sample of such perovskite solar cells has an efficiency of 2,62%. An opportunity for the use of a ZnO:B film as an inexpensive substitute for transparent conductive oxides such as FTO and ITO substrates was shown.

Optical Materials and Devices

Nanoscience

Energy Engineering

Physical Chemistry

perovskite solar cell

ZnO film

LPCVD

transparent conductive oxides

Perovskite solar cells (PSCs) are a very intensive and popular topic of research in the last decade in the field of photovoltaics (PVs). This capability is connected with the potential of these materials to produce low-cost and high-efficiency solar cells [1–4]. Among PSC structures with n-i-p design architectures, n-layers, transporting light exiting electrons, harvesting light in the i-layer and hole conduction in the p-type layer are noticeable [5]. Electron-transportable n-type layers are used for the extraction of electrons excited by light and further transport. Additionally, at the same time, this layer is used for suppressing recombination processes between light-excited electrons and holes in bulk perovskite films [6].

Metal oxides, for example, titanium dioxide (TiO₂), tin oxide (SnO₂) and zinc oxide (ZnO), are widely available for use as electron-transport materials in the n-i-p design of perovskite solar cells [7]. Among the abovementioned types of metal oxides, TiO₂, perovskite, and Spiro-OMeTAD have good performance parameters [8–10]. A prospective material, ZnO, can also be interesting for its n-i-p perovskite structure because ZnO is a nontoxic material with a wide band gap and because the preparation of films uses affordable precursors; in addition, these films can be conductive due to their low resistivity [11],[12]. ZnO has a band gap of 3,37 eV, and its electrons have greater mobility than TiO₂ [13]. Thus, ZnO is used as an electron transporting layer (ETL) in PSCs [5],[14–16]. Since a layer can be formed at lower synthesis temperatures, this opens up the opportunity to form a layer on flexible substrates with low resistance and high transparency [7]. These advantages satisfy the requirements for a combination of qualities such as an affordable price and the possibility of an optimal combination of conductivity and transparency in transparent conductive oxide films [17–19]. In addition, ZnO can potentially be an alternative replacement for the wide use of ITO films in modern optoelectronic applications [20–23] because indium and gallium are rare elements with constantly growing costs, and the search for cheaper and more common materials is a relevant research direction [24]. The properties of ZnO can be modified by boron doping during film formation. This approach allows not only an increase in the free electron concentration but also impacts the crystallinity, roughness and optical properties of the material [25, 26]. Previously reported ZnO:B materials were used in zinc oxide and copper oxide ZnO:B/CuO solar cells (heterojunctions) [27–29], as TCO materials in amorphous and crystalline silicon solar cells [30–33] and in the 3rd generation of solar cells [6]; therefore, the application of these materials in new types of solar cells is an actual challenge.

In this work, the surface, structural, optical and electrical properties of ZnO:B films made by the low-pressure chemical vapor deposition (LPCVD) technique were studied. This procedure was used to evaluate the capability of the material for PSC formation. Additionally, a solar cell was made on the ZnO:B film. It was demonstrated that TCO layers based on indium and tin oxides can be replaced by ZnO:B layers in simple planar cell architectures (glass/ZnO:B/MAPI/Spiro-Ome-TAD/Au), and these materials can be effective for creating PSCs.

The surface, structural, optical and electrical properties of the ZnO:B film were studied, as was its influence on the properties of the solar cell.

The optical properties and transmittance coefficient in the wavelength range of 300–1100 nm were studied by a “QEX-10” device (PV Measurements, Inc.). A scanning electron microscope (JSM-6490LA) and an atomic force microscope (JSPM-5200-1) produced by Jeol were used for surface analysis. The electrical properties of the ZnO films were studied by means of a Hall Effect Measurement System (HEM-2000) produced by the “EGK Corporation”.

X-ray analysis of the substrate base was performed using a “BRUKER D8 Discover” diffractometer (with a source of radiation CuKα). The analysis was performed with the Bruker suite, which included Diffrac. Eva, Topas, Leptos, and Diffrac. The crystallographic information was obtained from an online database.

Photoluminescence (PL) spectra were obtained using a CaryEclipse spectrophotometer (Agilent) in the wavelength range of 300–850 nm. The radiation of a pulsed xenon lamp was used for excitation. The excitation spectrum was corrected by a bandpass filter for a wavelength of 300 nm with a bandwidth of 27 nm. The scattered radiation of the xenon lamp was removed by an edge filter at a wavelength of 325 nm.

Structural properties

The ZnO:B layer was studied via XRD. The results of the research are shown in Fig. 1.

The predominant crystalline phase in the polycrystalline ZnO film is a hexagonal lattice of zinc oxide with the space group Pnma (62). The most important peaks at 31.8°, 34.4°, 36.2°, 47.5.40°, 56.6°, and 62.9° correspond to the ZnO planes, with the following orientations: (100), (002), (101), (102), and (110) и (103), respectively. The X-ray diffraction results are consistent with the standard database of nonorganic crystal structures of ZnO (ICDD 00-005-0664). Moreover, the high intensity of the (110) band indicates the texture and predominant orientation of the crystallites.

In addition to the zinc oxide phases, weak XRD signals are present in the XRD patterns of the ZnO sample at angles of 50.81° and 54.25°, which can be attributed to the (-129) and (-327) planes, respectively, of the zinc borate phase with a monoclinic crystal structure, which corresponds to the Zn₃(B₂O₆) database (ICDD 00-027-0983).

Surface morphology

Figure 2 shows scanning electron microscopy (SEM) images of the ZnO:B layer surface.

The sample surface consists of many pyramidal micro-objects with a predominant direction of growth along the (110) direction according to the XRD results in Fig. 1.

The surface of the ZnO:B sample was also studied by atomic force microscopy (AFM). The AFM image is shown in Fig. 3.

As shown in Fig. 3a, the maximum height of the objects on the surface is 494 nm at a scale area of 25x25 mcm². Generally, the surface is embossed, and the average roughness is Rs = 56 nm at a scale area of 25x25 mcm² and Rs = 57 nm at areas of 12, 5 х 12, and 5 mcm² (Fig. 3a). In addition to the AFM technique, the ZnO:B material was studied by SEM, and the cross-sectional image is shown in Fig. 3b. SEM scanning made it possible to measure the film thickness, which was 2 microns.

Optical properties

A study of the optical properties of the films was carried out in the wavelength range 300–1100 nm. Figure 4a shows the optical transmission spectra of a ZnO:B film on glass.

The average transmittance is 66% in the visual range (λ = 380–780 nm), with a total change in value from 3–77%. In the NIR range (λ = 790–1100 nm), the average value is 83%. In general, the film showed high transmission capacity at a thickness of 2 µm in the visible and near-IR regions. For the use of materials in solar cells as transparent conductive electrodes that do not require the creation of a contact grid, a throughput of approximately 66% in the visible region is sufficient.

The inset in Fig. 4a shows a graph for determining the band gap EG using the Tauc and Davis–Mott model [34],[35] where E_G was found to be 3.24 eV. This model was chosen because it is suitable for both amorphous and polycrystalline materials. The band gap of undoped zinc oxide films covers a wide range from ~ 3.1 to ~ 3.5 eV [36]. Similarly, the band gap of ZnO:B is somewhat greater than that of titanium oxide TiO2 (3.2 eV) [37], [38].

The PL spectrum of the initial ZnO films (Fig. 4b), measured at room temperature with excitation at a wavelength of 300 nm, consists of a near-band edge emission NBE with a maximum near 380 nm and a half-width of ~ 0.18 eV and a wide emission band through deep levels (deep-level emission DLE) in the region of 500–700 nm. The intensity of both the NBE and DLE emission bands varies somewhat from sample to sample. Since the intensity ratio of the NBE and DLE bands characterizes the concentration of nonradiative recombination centers, the predominance of interband radiation in samples with a high concentration of free carriers may indicate high crystallinity of the ZnO layers.

Electrical properties

Measurements of the electrical characteristics were carried out by the Hall effect method, and the concentration of charge carriers and the mobilities of free electrons in the ZnO:B semiconductor films were determined. The measured characteristics of the ZnO:B film are shown in Table 1.

Table 1

– Electrical properties of the ZnO:B film
Samole	Film thickness, mcm	Bulk charge carrier concentration, cm^-3	Mobility, cm²/V×s	Resistivity, Оhm×сm
ZnO:В	2	7.00×10¹⁹	35	2.50×10^− 3
ZnO:В [39]	2.2	1.20×10²⁰	30	1.70×10^− 3
ITO [40]	0.6	1.16×10²¹	30	1.80×10^− 3

The test sample has a lower concentration of charge carriers but has a higher mobility and a slightly higher resistivity than the measured parameters [39]: 7×10¹⁹ cm^− 3 versus 1.20×10²⁰ cm^− 3; additionally, the mobility is 35 cm²/V×s, and the resistivity is 2.5×10^− 3 Ω × cm versus 30 cm²/V×s and 1.7×10^− 3 Ω × cm. The ZnO:B film from the abovementioned reference paper was used in amorphous Si solar cells. The table also contains the parameters of ITO (indium tin oxide) films [40], for which the resistivity is approximately the same as that in the above article and in the sample studied in this work: 1.8×10^− 3 Оhm×сm versus 1.7×10^− 3 Оhm×сm and 2.5×10^− 3 Оhm×сm, respectively. ITO has the same resistivity but is more expensive due to the rarity of indium [41]. The analysis of these works makes it possible to set the required levels of values for application in photovoltaics in terms of the bulk concentration of charge carriers − 10²⁰, mobility – 10 ¹ and resistivity – 10 ^− 3. The relatively good electrical parameters of the studied ZnO:B sample allowed it to be used as a TCO substrate.

Making a Perovskite Solar Cell

The ZnO:B layer obtained by LPCVD was 3×3 cm² in size and was used as a substrate for PSCs. A perovskite solution (СH₃NH₃PbI₃-MAPI) consisting of dimethylformamide (Merck), dimethyl sulfoxide (Merck), methylammonium iodide (Dyesol/Greatcell) and lead iodide (Merck) was deposited on a ZnO:B substrate using a spinner. During the formation of the perovskite film during unwinding, ethyl acetate was added to accelerate the process of crystallization; after deposition, annealing was carried out at 100°C for 10 min. The p-type layer Spiro-OMe-TAD (Merck) was deposited on the spinner from a solution based on chlorobenzene with the addition of a solution of acetonitrile (Merck) and a Li-TFSI salt (Merck). Gold electrodes for the solar cell were obtained by thermal vacuum deposition on an Edwards 306 setup. The results of the study of the phase composition of the samples are shown in Fig. 5.

The main phase corresponds to a perovskite layer of lead methylammonium iodide with an orthorhombic lattice with space group Pnma (62). Additionally, the diffraction patterns show peaks attributed to the substrate of zinc oxides doped with boron. The results of X-ray diffraction analysis of the samples correspond to the standards of the database of inorganic crystal structures CH₃NH₃PbI₃ (ICDD 01-086-6112) and ZnO (ICDD 00-005-0664).

The performance study was carried out through the measurement of the current‒voltage characteristic (I–V curve), which was measured on a solar simulator "Newport Oriel Sol3A" with illumination mode AM 1.5. The measurement results are shown in Fig. 6.

The operating parameters of the IV curve of the perovskite solar cell on the ZnO:B film shown above are presented in Table 2.

Table 2 - Performance parameters of the perovskite solar cells on the ZnO:B film

No	Sample	V_oc,V	J_sc, mA/cm²	FF, %	PCE, %
1	glass/ZnO:B/MAPI/Spiro-OMeTAD/Au (planar-type)	0,51	11,22	45,41	2, 62

Here, is a planar sample on a ZnO:B film. This solar cell has a glass/ZnO:B/СH₃NH₃PbI₃/Spiro-OMeTAD/Au structure (Fig. 7).

Considering the planar-type structure, the efficiency of this type of perovskite solar cell is high enough. For example, solar cells in which a layer of ZnO was obtained from nanocoloids [42] demonstrated a maximum efficiency of 4.39%. Similarly, in [8], samples with a complex structure based on ITO and ZnO nanoparticles had an efficiency comparable to ours; an element with the ITO/ZnO/CH3NH3PbI3 perovskite/spiro-OMeTAD/Au architecture was fabricated, and a PCE = 2.9% was obtained at V_oc = 0.84 V, J_sc = 7.3 mA/cm², and FF = 47.6%. In [43], a cell based on ITO and ZnO nanorods had an efficiency of 2.18% at V_oc = 0.99 V, J_sc = 5.57 mA/cm², and FF = 39.58%. In our case, we demonstrate that the ZnO layer can act as both an electron-transport layer and a rear transparent conductive contact. A simple cell design based on ZnO:B without the use of expensive ITO layers holds promise for cost-effective perovskite solar cells.

The present work demonstrated the possibility of using boron-doped zinc oxide films in perovskite solar cells instead of TCO films based on indium and gallium oxides. The ZnO:B layer obtained by the LPCVD method can act as a transparent conductive contact and at the same time as an electron-transport layer for a perovskite light-absorbing material. The fabricated device structure glass/ZnO:B/MAPI/Spiro-Ome-TAD/Au showed an efficiency of 2.62%. To further increase the efficiency, it is necessary to optimize the thickness of the base layer in further studies.

Acknowledgments: The authors thank E.I. Terukov’s group of PTIs, named after Ioffe, for providing the ZnO:B samples. Special thanks to Konstantin Mit and Bagdat Rakymbetov for the AFM and SEM surface studies. Additionally, we express acknowledgments to Dr. Adam Pockett for his help in preparing perovskite solar cells in the Swansea laboratory.

Author contributions

Sultan Zhantuarov - prepared the text, comparing the experimental data with the literature data.

Prof. Matthew Carnie - foreign science supervisor of Sultan Zhantuarov, providing laboratory materials for the experiments.

Dr. Nurlan Tokmoldin - Science supervisor of Sultan Zhantuarov, author of idea to use ZnO:B films for perovskite solar cells.

Dr. Aigul Shongalova - XRD and optical plot processing and preparation.

Kairat Zholdybaev - Hall effect measurements and data interpretation.

Prof. Khabibulla Abdullin - PL-, XRD - spectral measurements and interpretation, article’s structural recommendations.

Dr. Kazybek Aimaganbetov - corresponding author, transmittance spectra measurements and optical and electrical property film interpretation, paper text analysis.

Funding: This research was funded by the Science Committee of the Ministry of Education and Science of the Republic of Kazakhstan (Grant No. AP22687885).

Competing interests: The authors have no relevant financial or nonfinancial interests to disclose.

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The authors declare no competing interests.

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Properties of a ZnO:B Layer Fabricated by LPCVD and Its Application in Perovskite Solar Cells

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