NiO-NiTiO3 Heterojunction for Enhanced Solar Cell Efficiency and Hydrogen Evolution: A Stable All-Oxide Approach

NiO-NiTiO3 Heterojunction for Enhanced Solar Cell Efficiency and Hydrogen Evolution: A Stable All-Oxide Approach | Authorea try { document.documentElement.classList.add('js'); } catch (e) { } var _gaq = _gaq || []; _gaq.push(['_setAccount', 'G-8VDV14Y67G']); _gaq.push(['_trackPageview']); (function() { var ga = document.createElement('script'); ga.type = 'text/javascript'; ga.async = true; ga.src = ('https:' == document.location.protocol ? 'https://ssl' : 'http://www') + '.google-analytics.com/ga.js'; var s = document.getElementsByTagName('script')[0]; s.parentNode.insertBefore(ga, s); })(); Skip to main content Preprints Collections Wiley Open Research IET Open Research Ecological Society of Japan All Collections About About Authorea FAQs Contact Us Quick Search anywhere Search for preprint articles, keywords, etc. Search Search ADVANCED SEARCH SCROLL This is a preprint and has not been peer reviewed. Data may be preliminary. 7 April 2025 V1 Latest version Share on NiO-NiTiO3 Heterojunction for Enhanced Solar Cell Efficiency and Hydrogen Evolution: A Stable All-Oxide Approach Authors : Kaushik GHOSH 0000-0003-1278-7587 [email protected] , Nikita Chaudhary , Ayushi Jain , Mansi Pahuja , Subhabrata Das , Jyoti Jyoti , Harini EM , … Show All … , Seema Rani , Shumile Siddiqui , Daya Rani , Mohd Afshan , Soumyadip Sharangi , and Chandan Bera Show Fewer Authors Info & Affiliations https://doi.org/10.22541/au.174405082.27081771/v1 353 views 172 downloads Contents Abstract Information & Authors Metrics & Citations View Options References Figures Tables Media Share Abstract Green energy production has become necessary in order to achieve sustainable development goals and transition towards a green economy where solar energy and hydrogen fuel serve as the forthcoming energy sources. In this aspect, perovskite materials find potential applications in the generation of green hydrogen as well as solar energy. While various halide and lead-based perovskites have shown promising results in photovoltaic technology, their stability and toxicity issues hinder the commercialization of the technology. NiTiO3 is a stable n-type perovskite oxide with a broad absorption range from UV to visible NIR range. However, the application of oxide perovskite materials has not been explored extensively. The creation of p-n heterojunction in NiO-NiTiO3 enhances photo-generated charge carrier separation. The interface offers a stronger interaction facilitated through Ti-O bond formation and a characteristic band gap of 1.27 eV, lower than the individual layers, facilitating charge transfer. This accompanied with the higher density of states in the heterojunction improved the efficiency of NiTiO3 based solar cell to 4.25% as compared to the previously reported 1.66%. Additionally, the all-oxide device provides 87% efficiency retention after six months. Exploring the versatility of this heterojunction, its application in green hydrogen generation has been studied, where the NiO-NiTiO3 thin film catalyst yielded an overall hydrogen production of 5.04 mmol g-1/1.68 mmol g-1 h-1 of the catalyst. Therefore, all oxide perovskite heterojunction serves as a prospective candidate for the advancement of renewable energy generation techniques. NiO-NiTiO 3 Heterojunction for Enhanced Solar Cell Efficiency and Hydrogen Evolution: A Stable All-Oxide Approach Nikita Chaudhary 1 , Ayushi Jain 1 , Mansi Pahuja 1 , Subhabrata Das 1 , Jyoti 1 , E M Harini 1 , Seema Rani 1 , Shumile Ahmed Siddiqui 1 , Daya Rani 1 , Mohd Afshan 1 , Soumyadip Sharangi 1 , Chandan Bera 1 , Kaushik Ghosh 1* 1 Institute of Nano Science & Technology, Knowledge City, Sector-81, SAS Nagar, Manauli P.O-140306, Mohali, Punjab, India. *Corresponding Author email: [email protected] Electronic Supplementary Information (ESI) available Abstract: Green energy production has become necessary in order to achieve sustainable development goals and transition towards a green economy where solar energy and hydrogen fuel serve as the forthcoming energy sources. In this aspect, perovskite materials find potential applications in the generation of green hydrogen as well as solar energy. While various halide and lead-based perovskites have shown promising results in photovoltaic technology, their stability and toxicity issues hinder the commercialization of the technology. NiTiO 3 is a stable n-type perovskite oxide with a broad absorption range from UV to visible NIR range. However, the application of oxide perovskite materials has not been explored extensively. The creation of p-n heterojunction in NiO-NiTiO 3 enhances photo-generated charge carrier separation. The interface offers a stronger interaction facilitated through Ti-O bond formation and a characteristic band gap of 1.27 eV, lower than the individual layers, facilitating charge transfer. This accompanied with the higher density of states in the heterojunction improved the efficiency of NiTiO 3 based solar cell to 4.25% as compared to the previously reported 1.66%. Additionally, the all-oxide device provides 87% efficiency retention after six months. Exploring the versatility of this heterojunction, its application in green hydrogen generation has been studied, where the NiO-NiTiO 3 thin film catalyst yielded an overall hydrogen production of 5.04 mmol g -1 /1.68 mmol g -1 h -1 of the catalyst. Therefore, all oxide perovskite heterojunction serves as a prospective candidate for the advancement of renewable energy generation techniques. Keywords: perovskite, hysteresis, fill factor, power conversion efficiency, solar energy. Introduction World has reached a consensus on the essentiality of transitioning from conventional sources of energy towards renewable and green energy sources in order to meet the goals of Paris Agreement, 2016 1,2 . Considering the recent trends of the world’s energy consumption, solar energy plays a significant role in meeting daily electricity needs 3 . While the total global energy requirement is 0.584 ZJ per year, Sun provides 725 ZJ of energy every year 4 . Therefore, harnessing solar energy can help in sustainably meeting the present energy demand. The first-generation crystalline silicon cells hold a staggering 75% of the market share in the solar sector 5 . However, they require laborious, expensive and advanced fabrication techniques increasing the overall cost of fabrication. Kojima et al. established a new category of solar cells in 2009 which provided a power conversion efficiency of 3 – 4% using ABX 3 perovskite type active materials 6 . These third-generation materials provide the benefits of easy fabrication, cost-effectiveness and high efficiency 7 . Within a short span of time, the power conversion efficiency has exceeded 20 % comparable to the commercially available silicon solar cells 8 . Lead based perovskites yield high efficiency perovskite solar cells (PSCs) with their appropriate band gaps, high absorption efficiency, long charge diffusion lengths and long charge carrier lifetimes 9 . Yet this technology is facing commercialization issues owing to various issues including toxicity, stability, volatility of organic compounds and large-scale fabrication 10,11 . Various degradation factors including humidity, light, heat and magnetic fields affected the performance of the devices 10,12 . The current research focus, therefore, shifted towards replacing lead with materials like tin (Sn), germanium (Ge), bismuth (Bi) and antimony (Sb) for creating non-toxic counterparts like tin halide perovskites, double perovskites, rudorffites etc. 13 . However, lattice distortions due to their unstable lattice structures, poor carrier transport, non- radiative recombination and self-trapping lead to poor power conversion efficiency 14 . While different perovskites have shown considerably power conversion efficiency, yet their low stability remains the most challenging factor in their commercialization. Comprehensive strategies like additive engineering, use of buffer layer, optimization of electron and hole transporting layer as well encapsulation have been explored to enhance the stability of PSCs [15,16]. The reactive nature of perovskites pose a serious challenge towards the stability of the device due to its reactive propensity towards oxygen, charge transport layers as well as with the metallic contacts 17,18 . On the other hand, oxide materials have less reactivity towards atmospheric moisture and are highly stable while providing broad range absorption along with band gap tunability. While many oxides have found their applications as ETL and HTL (SrTiO 3 19 , PbTiO 3 20 ) layers in PSCs, their applications as active layers not extensively explored. A German scientist, Gustav Rose in 1839 discovered perovskite oxides from a mineral CaTiO 3 . Structurally similar titanium based perovskites of MTiO 3 (M = Ba, Sr, and Ni) have been widely explored in photocatalytic studies 21 . Among these, Nickel titanate (NiTiO 3 ) has recently attracted attention towards its applications in hydrogen generation and green energy production due to its stability in oxidizing environments 22 . It is an n-type semiconductor material having an octahedral combination of nickel and titanium, exhibiting an ilmenite structure. It has a broad absorption range covering from UV to near IR region having a tunable band gap of 2.2 eV – 2.7 eV. These properties make it an ideal candidate for serving as an active layer in photovoltaic devices. However, high charge recombination rates in oxides pose serious challenges for their applications in such devices. Yet, this issue can be addressed the by creation of suitable Type-II band aligned heterojunction. Li et al. has reported a similar heterojunction of NiTiO 3 with TiO 2 nanowires to design a dye-sensitized solar cell, where this perovskite served as a sensitizer layer and p-n heterojunction formation enhanced the efficiency of from 0.75 % to 1.66 % 21 . Therefore, NiTiO 3 finds potential applications as active material in perovskite solar cells. This report aims to develop NiTiO 3 active layer based all oxide perovskite solar cell xhibiting high efficiency and stability. To create a low cost device, NiTiO 3 has been synthesized using a simple CVD method while NiO nanoparticles have been synthesized using solution based method. The charge separation in this heterojunction has been confirmed via time correlated single photon counting (TCSPC) study. To design a photovoltaic device, spin-coating has been used followed by low temperature annealing. In order to achieve an open circuit voltage, a tin oxide based electron transport layer has been utilized rather than traditional TiO 2 ETL that requires high temperature processing very low valence band of SnO 2 and a very high conduction band of NiO layer ensures an efficient charge transfer from NiTiO 3 to the ETL and HTL layers. The as-fabricated device has been studied for its photovoltaic behavior using AM 1.5 G conditions. Further, the device characteristics have been studied under forward and reverse scan characteristics to quantify the hysteresis behavior, usually observed in perovskite solar cells 23 . Various reasons leading to the hysteric behavior have been explored and the number of defect states (5.2 x 10 13 cm -3 ) have been quantified using the space charge limited current (SCLC) region analysis, which is found to be much lower than the recent reports on oxide perovskite system. The major attraction of this device is its long-term stability for a period of six months which may be attributed to the chemical robustness of oxide materials against open environmental conditions. Additionally, NiO-NiTiO 3 heterojunction is found to be very suitable towards the hydrogen evolution reactions in 0.1 M Na 2 SO 4 solution with considerably low overpotential and significantly long stability for 7 hours in neutral medium under illuminated conditions. Photo-response characteristics of the as designed electrode has been estimated with a distinct improvement in onset potential @ 3 mA cm -2 from 1.01 V under dark conditions to 0.766 V under light irradiation leading to an impressive production of green hydrogen of 5 mmol/g of catalyst loading at 3 hours of continuous light illumination. LSV curves for the heterojunction have been observed under dark and light conditions followed by quantification of hydrogen production using gas chromatography technique. In nutshell, the NiTiO 3 based heterojunction has been explored to unveil the potentiality of oxide-based perovskites towards renewable energy harvesting and storage. Results and discussion XRD and SEM analysis The X-ray diffraction technique has been utilized to characterize the crystallinity and the uniform particle size of the as-prepared NiTiO 3 , NiO and SnO 2 as shown in Fig. 1a and Fig S1, respectively 24 25 . The XRD pattern of NiTiO 3 confirms the diffraction peaks at 24.1, 33.1, 36.6, 53.9 and 49.4 corresponding to (012), (104), (110), (116) and (024) planes (JCPDS No. 01-075-3757) respectively. The highest peak at 33.1 represents the rhombohedral structure with lattice parameters a = b = 5.0321 Å and c = 13.7924 Å indicating successful synthesis of ilmenite phase of this perovskite. The XRD peaks of the perovskite are found to be different from the precursor material indicating a successful synthesis of the desired active material. The average crystallite size of both materials have been calculated using the Debye Scherrer equation given as D = Kλ/β cos θ, where K is Scherrer constant (0.98), λ is the wavelength (1.54), β is full width at half maximum (FWHM) and θ is Bragg’s angle and the crystallite size for NiTiO 3 is calculated to be 55.5 nm. The XRD pattern. Similarly, the XRD pattern of NiO nanoparticles (Fig. S1b) demonstrates diffraction peaks at 43.2 (200), 37.2 (111) and 62.8 (220) belonging to JCPDS No. 00-047-1049. The as-synthesized NiO nanoparticles exhibit cubic phase indicating Bunsenite structure. Fig. 1: (a) XRD pattern of NiTiO 3 and precursor mixture of NiO and TiO 2 confirming the formation of perovskite material, SEM image of (b) Mesoporous SnO 2 thin film over FTO substrate, (c) NTO thin film coated above SnO 2 layer, (d) NiO thin film coated over NTO, and (e) Lateral view of the photovoltaic device. The photovoltaic device performance of thin film oxide heterojunction is widely dependent on its morphological appearance, which is precisely characterized by field emission scanning electron microscopy (FESEM) technique shown in Fig 1. Fig. 1b depicts the SnO 2 thin film decorated on FTO surface exhibits a porous architecture with the presence of multiple well-like ditches morphology whereas the uneven morphology has been controlled with a secondary coating of NiTiO 3 thin film over SnO 2 ETL layer (Fig. 1c). The granular architecture of this nanoparticle based thin film shows the formation of particles having uniform size distribution with wide coverage over the underlying layer. The porous and granular nature of both these layers have helped in interlinking of the active material with ETL layer. These grain boundaries are responsible for the hysteric behaviour of the device (as discussed later). Finally, a compact HTL layer comprising of NiO particles has been decorated on the active material surface with a minimized pinhole morphology, shown in Fig. 1d. Finally, Fig. 1e. shows the lateral view the device with clear differentiation between each component (Mapping shown in Figure S2). Further, X- ray photoelectron spectroscopy (XPS) has been performed for analysing the elemental composition of the materials. The XPS survey spectrum (shown in Fig. S3) of NiTiO 3 confirms the elemental composition of the perovskite including Ni, Ti and O elements. The surface chemical states of NTO has been examined where the high-resolution Ni 2p spectrum (shown in Fig. 2a) has been de-convoluted into peaks positioned at 855.44 eV, 872.93 eV indexed to 2p 3/2 and 2p 1/2 states of Ni 2+ with their respective satellite peaks at 861.71 eV and 879.79 eV 24 , respectively. The high-resolution Ti 2p spectrum (shown in Fig. 2b) has been de-convoluted into peaks positioned at 458.1 eV and 463.8 eV corresponding to 2p 3/2 and 2p 1/2 states respectively. The oxygen 1s peak (shown in Fig. 2c) has been de-convoluted into two peaks, first at 529.82 eV corresponding to lattice oxygen (O 2- ) in Ni-O and Ti-O bonds and the second peak at 531.5 eV corresponds to oxygen vacancies in the material. The ratio of Ov/O L comes out be 0.216 responsible for giving rise to additional electronic states near the conduction band of NTO 26 . Similarly, the elemental compositions of SnO 2 and NiO have been confirmed using XPS, as shown in Fig. S4,S5 respectively. Fig. 2: High resolution XPS profile of (a) Ni (2p), (b) Ti (2p), and (c) O (1s) in NiTiO 3 . Optical Characterization The optical characterization of NiTiO 3 thin has been performed using UV-Vis Diffuse Reflectance Spectroscopy (DRS) shown in Fig. 3a. The major absorption peaks have been identified at 315 nm, 464 nm and 744 nm. The band gap of NTO has been calculated using the corresponding Tauc plot shown in Fig. 3b. indicating the presence of two band gaps at 2.23 and 2.44 eV which are in agreement with the reported literature 27,28 . The absorption spectra and the corresponding Tauc plots have studied for SnO 2 and NiO as well (shown in Fig. S6). Further, to understand the charge carrier dynamics between the perovskite thin and NiO thin film, photoluminescence (PL) spectroscopy has been performed. The PL graph in Fig. 3c shows the quenching of the PL intensity in the heterojunction thin film indicating a charge extraction with the application of NiO. To confirm this finding, time correlated single photon counting (TCSPC) analysis has been investigated as shown in Fig. 3d. The average charge carrier lifetime of NTO calculated from PL spectroscopy is 12.93 ns which is similar to organic lead halide perovskite (MAPbBr 3 ) 29 . The decrease of average charge-carrier lifetime to 7.96 ns in NTO-NiO heterojunction is in resonance with the PL spectroscopy 30 . The thickness of the NiO HTL layers has been optimized in order to get the maximum conductivity for faster charge transport (shown in Fig. S7). Therefore, the fabrication of a device based of NTO-NiO heterojunction would improve the charge carrier separation. Fig. 3: (a) Absorbance spectra and (b) Tauc plot of NiTiO 3 , (c) Photoluminescence spectra and (d) Time correlated single photon counting (TCSPC) spectra of NiTiO 3 and NiO-NTO heterojunction. With respect to the device fabrication of a photovoltaic, band alignment of various layers in the device has been confirmed using ultraviolet photoelectron spectroscopy (UPS) to calculate the conduction and valence band positions. Fig. 4a. shows the UPS spectra for NiTiO 3 and Fig S8 shows the UPS spectra for SnO 2 and NiO respectively. The Type II band alignment of the active layer along with ETL and HTL layers allow the facile charge carrier transport as shown in Fig. suitable for a photovoltaic device. Additionally, a very low valence band of SnO 2 with respect to NTO and a very high conduction band of NiO with respect to NTO provide an efficient electron-hole separation (depicted in Fig. 4b.) along with low possibilities of recombination. Fig. 4: (a) UPS spectra of NiTiO 3 and (b) Type-II band alignment of solar cell layers at equilibrium, showing band offset leading to hole accumulation. Photovoltaic performance: An all oxide based perovskite solar cell has been fabricated (discussed in experimental section) having device structure: FTO/SnO 2 /NTO/NiO/Au (shown in Fig. 5a.). The J-V characteristics of the designed device in both forward and reverse directions have been shown in Fig. 5b. It can be observed that the short circuit current density (J SC ) is -13.67 mA cm -2 in reverse direction and -13.32 mA cm -2 in the forward direction, whereas the open circuit voltage (V OC ) is -0.4 V and 0.385 V respectively. In both directions, J SC and V OC are nearly similar, therefore, fill factor (F.F.) will be the deciding factor for the power conversion efficiency (PCE, η) given as: F.F. = ( J m *V m )/( J sc *V oc ), (2) Where J m and V m are the current and voltage, respectively, at maximum power point of the J-V curve. The fill factor is 0.68 in reverse direction as compared to 0.83 in the forward direction. Thus, the power conversion efficiency under AM 1.5 conditions is calculated as, ɳ (%) = (FF *J sc *V oc )/ P in (3) where, P in is the incident power of the input light, i.e., 100 mW/cm 2 . The PCE is found to be 4.25 % in forward direction as compared to 3.64 % in the reverse direction. The difference in the current characteristics with change in bias direction indicates the presence of hysteresis. This can be quantified using hysteresis index (HI) given as: HI= (PCE For – PCE Rev )/PCE For (4) The HI for the designed solar cell is 0.14 showing an normal type of hysteresis characteristics. 23 . Further, the stability for the device has been studied for 6 months in an ambient environment (shown in Fig. 5c). This all oxide device shows a PCE retention upto 87.1 % with a PCE of 3.7 % after 6 months. The oxide based thin films provide higher stability of the device in ambient conditions, which is a deteriorating factor for other organic and halide-based perovskites. Therefore, the suitable hetero-interfaces of the oxide-based material is found to be an accurate choice of photoactive template to design stable, reliable, and cost-effective renewable energy device. Fig. 5: (a) Device design of the solar cell depicting charge transfer mechanism, (b) J-V characteristics in forward and reverse directions, and (c) Stability of device performance. DFT results of NTO-NiO heterojunction: We have performed DFT calculations to complement our experimental observations. The side view of optimized NiO-NTO heterojunction is shown in Fig 6a. To reduce lattice mismatch, the (001) plane of NiO and the (110) plane of NiTiO 3 have been utilized, which contains a total of 132 atoms. The strong interaction between the NiO layer and the NiTiO 3 layer is evident in this combined structure. As illustrated in Fig 6a, there is a significant interaction between the Oxygen (O) and Titanium (Ti) at the interface of the two layers, which causes the Ti-O bond to shorten from 3.33 Å in the theoretical model to 2.06 Å in the optimized structure as depicted with black dotted circle. Fig 6(b) and 6(c) represent the projected density of states (PDOS) for pristine NiO and pristine NiTiO 3 , respectively. In Fig 6(b), the valence band maximum (VBM) of NiO is predominantly formed by O 2p-orbitals, whereas the conduction band minimum (CBM) is largely composed of Ni 3d-orbitals. In the case of NiTiO 3 , VBM is mainly dominated by O 2p-orbitals and CBM features a hybridization of Ti 3d and Ni 3d-orbitals as shown in Fig 6(c). The band gaps are calculated to be 2.96 eV for NiO, 2.14 eV for NiTiO 3 . Fig 6(d) displays the total density of states for the NiO-NTO heterojunction, which features a band gap of 1.27 eV. The reduction in band gap of the heterojunction is expected to improve the conductivity of the NiO-NTO complex, facilitating better electron transfer. To obtain qualitative insights into the electronic structure of the interface and identify the nature of the orbitals, PDOS for the NiO-NTO heterojunction is examined. Fig 6(d) shows that the VBM of the NiO-NTO heterojunction is occupied by the atomic orbitals of NiO, while the atomic orbitals of NiTiO 3 are positioned lower. The VBM of the heterojunction is predominantly influenced by O 2p-orbitals, as illustrated in Fig 6(e). In contrast, the CBM of the heterojunction is mainly occupied by the atomic orbitals of NiTiO 3 , with the atomic orbitals of NiO positioned higher than NiTiO 3 . The CBM is mainly composed of Ti 3d orbitals as shown in Fig 6(f). Since, the strong interaction between Ti and O atoms leads to a redistribution of electronic states and alters the relative positioning of Ti atoms, resulting in a significantly smaller band gap for the heterojunction compared to that of NiO and NiTiO 3 . While this band gap calculation cannot be directly correlated with the bulk materials studies because only single layers have been considered here for DFT calculations, the Ti-O bond formation reveals the generations of extra density of states in this heterojunction. Fig. 6: (a) Side view of optimized NiO-NTO heterojunction, (b) PDOS of NiO and, (c) of NTO by GGA+U methods, (d) TDOS and PDOS of NiO-NTO heterojunction, (e) PDOS of NiO in NiO-NTO heterojunction, and (e) PDOS of NiTiO 3 in heterojunction. Hysteric Behaviour: To understand the hysteric behaviour of the as-designed device, J-V characteristics of NTO thin film have been studied as shown in Fig. 7a. Usually, hysteresis is more prevalent at higher scan rates and is reduced at low scan rates. However, in NTO, the behaviour remains same at 20 mV/s and 200 mV/s scan rate indicating an inherent hysteric behaviour of the perovskite. This could be correlated with the ferroelectric nature of the material where the polarization of the material could not be completely reversed by changing the bias direction 31 . Secondly, the presence of oxygen vacancies at the junction interface serve as trap centres, usually the deep level traps, leading to the occurrence of hysteric behavior 32 . The existence of oxygen vacancies on the surface of NTO thin film and both charge transport layers is evident in XPS spectra shown in Fig. 2c, The trap filling and emptying process as well as charge recombination can cause higher hysteresis behavior 33 . To verify the number of trap states present in the system, the space charge-limited current (SCLC) for the photovoltaic device has been studied (shown in Fig. 7b). At V TFL , i.e., trap filling voltage limit, the value of current starts to increae at a higher rate. This value of V TFL has been utilised to calculate the trap-state density (N t ) in the system according to the following equation: \(\text{\ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ }N_{t}=\frac{\left(2\varepsilon_{0}\varepsilon_{r}V_{\text{TFL}}\right)}{\mathbb{e}L^{2}}\ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ \ (5)\) where, \(\varepsilon_{0}\) is the vaccum permittivity of free space (8.854 x 10 -12 F m -1 ),\(\varepsilon_{r}\) is the relative dielectric constant of the perovskite, e is electron charge and L is the thickness of the perovskite 30 . Here, the relative dielectric constant of NTO is 3.27, calculated using C-V graph shown in Fig. S9 34 . The total number of traps states in the system are found to be 5.2 x 10 13 cm -3 leading to the hysteric behaviour. Additionally, charge accumulation at the interface of ETL and HTL layer can lead to hysteresis. The band-bending diagram of solar cell junction has been shown in Fig. 4c. The higher energy offset of 0.72 eV at the NiO-NTO junction as compared to 0.64 eV at the SnO 2 -NTO heterojunction suggest the possibility of higher hole accumulation near the NiO layer 35 . Apart from these factors, the crystallinity and grain boundaries of the perovskite layer also contributes to the hysteric behavior. The nanoparticles based perovskite thin film have high number of grain boundaries (shown in Fig. 1c). Large amount of grain boundaries lead to higher hysteresis as compared to single crystals 36 . Therefore, hysteresis management becomes utmost important to improve the power conversion efficiency of all oxide perovskite based solar cells. Fig. 7: (a) I-V measurements of NiTiO 3 in forward and reverse directions and (b) SCLC measurements of the overall device. Hydrogen Evolution Reaction: The NiO-NTO heterojunction has been shown to have photoresponsive nature. The photo excitation of semiconductor material to create electron-hole pairs finds application in hydrogen generation. Therefore, this heterojunction has been studied for photocatalytic green hydrogen synthesis. Electrons are required to be present at the surface of the catalyst for HER to take place, thus, the as-fabricated catalyst structure is considered to be FTO/NiO/NTO. The performance of this thin film-based catalyst has been studied in neutral medium (0.1 M Na 2 SO 4 ) at a scan rate of 10 mV s -1 in a three-electrode system and the corresponding LSV curve has been shown in Fig. 8a. The increase in current has been observed with the application of NiO-NTO p-n heterojunction via efficient charge separation. The incidence of visible light on the heterojunction further enhances the current density through photo-generated charge carriers. The effect of light has been investigated using dynamic voltage study through Chrono potentiometry @ 18 mA cm -2 . A clear change in voltage has been observed (shown in Fig. 8b) when light is switched on and off confirming the presence of photoresponsive behaviour. The presence of oxygen vacancies in the perovskite and defect states serve as adsorption centres for H + ions leading to the formation of capacitive double layer at the electrode-electrolyte interface. The photo-response characteristics of the as designed electrode has been estimated with a distinct improvement in onset potential @ 3 mA cm -2 from 0.93 V under dark conditions to 0.6 V under light irradiation. To quantify the amount of H 2 being produced, the gas chromatography technique has been utilized as shown in Fig. 8d. Since, the loading percentage in these samples is very low (nearly 3 mg weight percentage of active material), the amount of hydrogen production is calculated to be 5.04 mmol g -1 /1.68 mmol g -1 h -1 (15.16 µmol cm -2 ) within 3 hours which is found to be nearly double than the recent findings on similar perovskite oxide based thin-film heterojunction 37 . To analyse the effect of incident light on the charge transfer properties of the catalyst, EIS Nyquist plots (shown in Fig. 8e) have been studied. The charge transfer impedance at the electrode-electrolyte surface is represented by the semi-circle in this graph, which gets reduced after light illumination. Thus, the EIS curves aligns well with the increase in current density in the presence of light where the R CT value decreses from 142 Ω to 85 Ω in the presence of light. At last, the chrono-potentiometry technique has been used to study the stability of the catalyst performance in the presence of light. The catalyst has been found to be stable upto 7 hours under illuminated conditions as shown in Fig 8f. The overall performance of the as-designed catalyst can be further increased by increasing the loading percentage or by utilising porous substrates providing higher surface area for photocatalytic activity. Fig. 8: (a) LSV curves in alkaline medium, (b) Chrono potentiometry curve showing dynamic light response, (c) LSV curves after 500 cycles, (d) Amount of hydrogen produced vs time curve using Gas Chromatography technique, (e) EIS Nyquist plot under dark and light conditions, and (f) Stability curve of the catalyst under light conditions. This report explores the application of all oxide heterojunction in renewable energy conversion and storage. In the areas of photovoltaic applications, it has been found that (a) nanoparticle-based thin films leads to cost-effective and ease of device fabrication, (b) the formation of Type-II band-aligned heterojunction leads to an efficient charge transfer mechanism, (c) the application of chemically stable oxide materials increase the overall stability of the device, and (d) optimized charge transport layers along with the active material creates an efficient photovoltaic device with a fill factor of 83 % and a power conversion efficiency of 4.25 %. The detailed understanding of the device performance has been further realised by its intrinsic hysteric behaviour originating through various factors: (a) the inherent polarization properties of the perovskite material, (b) large number of grain boundaries appearing via low-cost fabrication process, (c) the presence of oxygen vacancies along with the defect states, and (d) possibilities of hole accumulation at the NTO-NiO interface etc. Furthermore, the photoresponsive behaviour of NTO-NiO half-cell finds applications in green hydrogen generation, where the photo-induced charge carriers significantly enhance green hydrogen production. Therefore, these facile hetero-interfaces impart potential applications in the development of highly stable and effective solar-integrated hydrogen production and serve as suitable template for photovoltaic device to meet the increasing demand for renewable energy utilization. Conclusion: In summary, this report explored the application of oxide perovskites in developing stable and efficient photovoltaic technology. The chemical stability of oxide based active absorber layer provides a non-toxic alternative for the environmentally unstable organic-inorganic halide perovskite materials. In this aspect, the as-designed FTO/SnO 2 /NTO/NiO/Au device has shown impressive results compared to the recently reported oxide based counterparts with a 1.5-1.76 times higher fill factor and comparable efficiency owing to the optimal band alignment with both charge transport layers and higher number of density of states at the heterojunction resulting in superior stability over 6 months. Further, the utilization of the FTO/NiO/NTO template for hydrogen generation provides versatility to the heterojunction, where cumulative production of green hydrogen from thin film perovskite architecture is found to be nearly double, with reasonable good stability as compared to the recent reports. Therefore, deeper insights into the electronic structure at the interface of oxide based heterojunction and layer by layer optimization of device, indeed, can lead to the development of new class of perovskite oxide based photovoltaics as well as designing a thin film photocatalyst towards the development of sustainable technology, lucrative towards industrial adoption. Experimental Section: Synthesis of NiO nanoparticles: A 5 M solution of nickel nitrate hexahydrate (Ni(NO 3 ) 2 .6H 2 O) was prepared in distilled water. A 10 M solution of NaOH was mixed in the as-prepared nickel nitrate solution till the pH became 10. The precipitate was rinsed using deionized (DI) water and then collected by centrifugation followed by drying at 70° C. The dried sample was calcinated in muffle furnace at 300° C. The obtained powder was used to make NiO ink, i.e., 20 mg powder in a in a 7:3 volumetric solution solution of ethanol and DI [1] . Similarly, SnO2 nanoparticles were synthesized using hydrothermal method. SnCl 2 .5H 2 O solution was mixed with DI water and 2-propanol in volumetric ratio of 1:4.Later, a solution of NaOH is added to tis mixture to get the the pH value of 10. This was then kept in autoclave and heated for 24 hours at 150 °C [2] . Synthesis of NiTiO 3 nanoparticles: The perovskite nickel titanate was prepared by mixing nickel oxide (as prepared) with titanium oxide (TiO 2 ) nanoparticles in equimolar ratios. This mixture was grinded for 10 minutes to prepare a uniform mixture. This precusror was calcinated at 900 °C for two hours in a tubular furnace in ambient conditions. The as-obtained NiTiO 3 powder was grinded again for preparing ink for creating perovskite thin film. 50 mg of NiTiO 3 was dissolved in a 7:3 volumetric solution solution of ethanol and DI followed by 15 minutes of ultrasonication. Solar Cell Fabrication: For device fabrication, a Flourine-doped Tin Oxide (FTO) substrate was subjected to cleaning using isopropyl alcohol (IPA) and acetone followed by exposure oxygen plasma for 1 min to clean and activate the surface for enhancing thin film adhesion. A thin layer of SnO 2 nanoparticles was spin-coated on FTO at 3000 rpm for 30 s followed by baking at 200 °C on hot plate. Further, NiTiO 3 was spin-coated at an optimised rpm of 1500 for 45 s followed by 200 °C baking to get a better adhesion of the active layer with uniform film morphology. Lastly, NiO layer was spin-coated at 2000 rpm for 30 s with a sequential baking at 200 °C. The 100 nm silver (Ag) electrode was deposited via electron beam deposition at high vacuum conditions. A device configuration of FTO/SnO 2 /NiTiO 3 /NiO/Ag was fabricated having a total active area of 0.8 cm 2 . Photocathode fabrication: For photocathode fabrication, firstly Flourine-doped Tin Oxide (FTO) substrate was subjected to cleaning as described above followed by NiO film coating at 1500 rpm for 30 s followed by soft baking at 200 °C. Further, the active layer of NiTiO 3 was spin coated at 1500 rpm for 45 s with a 200 °C baking, resulting in the formation of uniformly decorated photocathode towards green hydrogen synthesis. Characterizations: The phase of the synthesized materials has been confirmed by powder X-ray diffraction (PXRD) using Cu Kα radiation (Bruker, eco D8 ADVANCE). The surface morphology of thin films has been investigated using field emission scanning electron microscopy (JEOL JSM-7600F) facility. The elemental composition has been studied using X-ray Photoelectron Spectroscopy (XPS) carried out via K-Alpha plus XPS system by Thermo Fisher Scientific instruments (Al Kα) having radiation energy 1486.6 eV at 5×10 -10 Torr ultra-high vacuum. The density of states study has been carried out using UV photoelectron spectroscopy (UPS) with He I excitations having energy 21.2 eV at a constant pass energy of 5 eV in ultra-high vaccum chamber of the XPS instrument. Shimadzu UV-2550 spectrophotometer has been used to record diffuse reflectance UV-Vis (DR UV-Vis) spectra. The photoluminescence study has been carried out using Fluorolog 3-221 fluorimeter. The time-correlated single photon counting (TCSPC) study has been carried out using a Deltaflex modular fluorescence lifetime system (HORIBA Scientific). The amount of H 2 produced by the photocathode has been measured under gas chromatography analysis (Shimadzu-GC-2014). The photovoltaic performance has been measured at room temperature under ambient conditions using Keysight B1500A semiconductor device analyser attached with AM 1.5G solar simulator having the power density of 100 mW cm -2 . Electrochemical Measurements: All electrochemical measurements have been carried out on an electrochemical workstation namely Metrohm-Autolab PGSTAT302N using three-electrode conFiguration. Platinum (Pt) wire has been used as counter electrode (Metrohm) and Ag/AgCl is taken as reference electrode, saturated with 3M KCl. The dissolved gases have been removed from the 0.1 M Na 2 SO 4 electrolyte via Argon purging for 30 minutes. LSV curves have been recorded to study the HER activity at a scan rate of 10 mV/s. Finally, Nernst equation has been utilized to transform the potential value to reversible hydrogen electron (RHE): E Ag/AgCl = E RHE - 0.197 - 0.059 x pH Computational Methods: All first-principles calculations are carried out using density functional theory (DFT) as implemented in the Vienna ab initio Simulation Package (VASP) [3] . The projector augmented wave (PAW) method is employed, and the exchange-correlation interaction is modelled using the Perdew-Burke-Ernzerhof (PBE) formulation [4,5] . Electronic wave-functions are represented with a plane-wave basis and a kinetic energy cut-off of 500 eV. Convergence criteria for energy and force are set at 10−6 eV and 0.02 eV/Å, respectively. Monkhorst-Pack grids of 3 × 2 × 1 are used for NiO, NiTiO 3 , and the NiO-NTO heterojunction. A vacuum layer of 18 Å is included along the z direction to prevent interactions between periodic images. The density of states is computed using GGA-PBE. To account for the correlation effects of localized d electrons, the GGA+U functional is applied, with on-site Coulomb parameters as U = 7.6 eV for Ni in NiO [6] and U = 3.5 eV and 4.5 eV for Ti and Ni in NiTiO 3 [7] , respectively. Author Contributions The manuscript was written through contributions of all authors. All authors have given approval to the final version of the manuscript. Conflicts of interest: None of the authors have any competing personal relationship of financial interest that could have influenced the work presented in the paper. Acknowledgements: K.G. is thankful to Ministry of Textiles [Grant 2/3/2021-NTTM(Pt.)] and N.C. is thankful to CSIR, New Delhi, India [Grant No.-09/1129(13373)/2022-EMR-I] for financial support. The authors also thank the Institute of Nano Science and Technology, Mohali, India, for use of their research facility. S.R. is thankful to CSIR, New Delhi and D.R., Jyoti are thankful for UGC, New Delhi for financial support. 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Information & Authors Information Version history V1 Version 1 07 April 2025 Copyright This work is licensed under a Non Exclusive No Reuse License. Keywords fill factor hysteresis perovskite power conversion efficiency solar energy Authors Affiliations Kaushik GHOSH 0000-0003-1278-7587 [email protected] Institute of Nano Science and Technology View all articles by this author Nikita Chaudhary Institute of Nano Science and Technology View all articles by this author Ayushi Jain Institute of Nano Science and Technology View all articles by this author Mansi Pahuja Institute of Nano Science and Technology View all articles by this author Subhabrata Das Institute of Nano Science and Technology View all articles by this author Jyoti Jyoti Institute of Nano Science and Technology View all articles by this author Harini EM Institute of Nano Science and Technology View all articles by this author Seema Rani Institute of Nano Science and Technology View all articles by this author Shumile Siddiqui Institute of Nano Science and Technology View all articles by this author Daya Rani Institute of Nano Science and Technology View all articles by this author Mohd Afshan Institute of Nano Science and Technology View all articles by this author Soumyadip Sharangi Institute of Nano Science and Technology View all articles by this author Chandan Bera Institute of Nano Science and Technology View all articles by this author Metrics & Citations Metrics Article Usage 353 views 172 downloads .FvxKWukQNSOunydq8rnd { width: 100px; } Citations Download citation Kaushik GHOSH, Nikita Chaudhary, Ayushi Jain, et al. NiO-NiTiO3 Heterojunction for Enhanced Solar Cell Efficiency and Hydrogen Evolution: A Stable All-Oxide Approach. Authorea . 07 April 2025. DOI: https://doi.org/10.22541/au.174405082.27081771/v1 If you have the appropriate software installed, you can download article citation data to the citation manager of your choice. Simply select your manager software from the list below and click Download. For more information or tips please see 'Downloading to a citation manager' in the Help menu . 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