CoSe2@N-Doped Graphene Nanocomposite High-Efficiency Counter Electrode For Dye-Sensitized Solar Cells

doi:10.21203/rs.3.rs-1197256/v1

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CoSe₂@N-Doped Graphene Nanocomposite High-Efficiency Counter Electrode For Dye-Sensitized Solar Cells

https://doi.org/10.21203/rs.3.rs-1197256/v1

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Photovoltaics is defined as a group of solar cells that convert solar energy into electricity. Among these cells, dye-sensitized solar cells (DSSCs) have received considerable attention due to of their low cost and high efficiency for energy conversion. In present study, CoSe₂@N-doped graphene nanocomposite has been prepared in an inert atmosphere and used as a DSSC counter electrode. The fabricated nanocomposite was characterised using analytical techniques including FTIR, TGA, XRD, Raman, XPS, and BET. The assembled DSSC obtains a photoelectric conversion efficiency (PCE) of 7.65%, which is higher than the PCE (7.19%) of the Pt electrode assembly cell under the same conditions. The promising performance of the fabricated counter electrodes may be due to the excellent surface area of the nanocomposites, the doping of hetroatomes which provide the active sites to boost the catalytic activities towards I₃^-reduction.

Dye-sensitized solar cell

Counter electrode

CoSe2

N-Doped Graphene

The sun has long been the most important renewable energy source on earth and the researchers are trying to utilize this vital source of energy for the benefit of humans. Even though, the world's biggest oil exporter, Saudi Arabia, has also pledged to cut its carbon emissions to net zero by 2060 and the plans and objective of Vision 2030, Saudi Arabia has focused on producing 50 percent of its electricity from renewable sources by 2030 to meet the growing demand for energy, and to provide favourable climatic conditions and suitable economic feasibility. Solar radiation can be converted directly into electricity by solar cells (photovoltaic cells) (Ahamad et al., 2021; Aldalbahi et al., 2021; Wang et al., 2021). Among these solar cells, dye-sensitized solar cells (DSSC) have attracted widespread attention due to their low cost, easy preparation, and high solar energy conversion efficiency (Hagfeldt et al., 2010; O'Regan and Grätzel, 1991). Generally, a typical DSSCs composed of a dye-adsorbed TiO₂ anode, a redox shuttle (I₃⁻/I⁻), and a counter electrode (CE). The function of CE is to collect the electron from the external circuit and catalyse the reduction of I₃ ⁻ into I⁻ (Jin et al., 2017; Leu et al., 2017; Meng et al., 2018). Pt is widely used as a counter electrode (CE) to fabricate DSSC due to its high conductivity and excellent catalytic activity towards I₃⁻reduction, however, the limited resources and high price of Pt limits its industrial application (Hou et al., 2018; Yu et al., 2016). Therefore, current studies are focused on finding alternatives to Pt. Some non-Pt materials such as porous carbon have been used as counter electrode to fabricate the DSSC due to their large surface area, high conductivity, and low cost (Tapa et al., 2021; Yue et al., 2018). Moreover, several transition metal based compounds specially, transition metal selenides, such as CoSe₂, NbSe₂, NiSe₂, and ZnSe₂ have excellent catalytic activity towards I₃⁻ reduction (Gao et al., 2018; Singh et al., 2017; Wang et al., 2016). Among these, cobalt selenide (CoSe₂) has attracted much attention because of its high catalytic activity, low cost and excellent long-term stability (Huang et al., 2018; Wang, X. et al., 2019; Yang et al., 2020). However, the electron conductivity of CoSe₂ is not meet to the required standard due to its semiconducting behaviour and poor conductivity (Chiu et al., 2016; Li et al., 2021; Ou et al., 2020). On the other hand, the carbon based materials such as graphite carbon, carbon nanotubes, graphene and graphene oxide not only show the excellent electrical conductivity but also the high surface area to enhance the catalytic activity. Recently, it was noticed that the doping of the heteroatoms such as N and S into carbon provide the additional active sites, which enhance the charge transfer behaviour as well as enhance the catalytic activity of the nanocomposites (Ding et al., 2022; Su et al., 2022; Wei et al., 2022). Therefore, the nanocomposite based counter electrode materials have attracted wide attention because they combine the advantages of each component and help improve the catalytic activity and the stability of the electrode (Silambarasan et al., 2021; Wang et al., 2022; Zhao et al., 2021). Being inspired by the above investigations, here we have design low-cost, effective and environmentally friendly counter electrode for DSSC using CoSe₂@N-doped graphene nanocomposite. The electrode materials were characterized using FTIR, XRD, Raman, BET, XPS, SEM and TEM. The electrochemical performance of CoSe₂@N-doped graphene was analysed by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV), and Tafel polarization curve, and the effects of N-doped graphene (NGN) loading with CoSe₂ were discussed in details. The DSSC fabricated using the CoSe₂/NGN-15 electrode exhibits excellent PCE value of 7.65% higher than that of other fabricated electrode even higher than that of the Pt electrode (7.19%) under the same experiment condition. This may be due to the synergetic effect between the CoSe₂ nanoparticles and graphene moreover the doping of the nitrogen into the graphene matrix also improve the DSSC performance and have good corrosion resistance to a corrosive redox electrolyte as CE materials. We hope that, the present work offers to fabricate Pt free counter electrode for DSSC and provides an opportunity to develop a highly efficient and low cost DSSC as the plans and objectives of Vision 2030.

2.1 Materials

Cobalt nitrate hexahydrate (Co(NO₃)₂·6H₂O, Graphene, selenium powder, N719 dye, are from Sigma-Aldrich. Ethylene glycol, Ethanol, Potassium iodide (KI), and Iodine (I₂) were obtained from Merck, Germany. TiO ₂ paste (TPP3, 20 nm; TPP200, 200 nm) and FTO glass (sheet resistance 15 Ω) were purchased from Dalian Seven Color Technology Co., Ltd.

2.2 Preparation of CoSe₂@NGN

The counter electrode materials were prepared as following; 20 mg of the NGN was dispersed into 50 mL ethanol and sonicated for 30 min., Then 0.40 mmol of Co(NO₃)₂.6H₂O and then 26 mmol (CH₃COO)Na were added to this mixture and stirred continuously. After that 0.80 mmol of SeO₂ was added to this solution and stirred again for 3 h, under N₂ gas, and then 4.92 mmol NaBH₄ dissolved in 20 mL ethanol was dropped to the above mixture and stirred overnight. The obtained precipitate was filtered, washed dried and then annealed at 400 ^oC for 4 h in N₂ atmosphere to remove amorphous selenium. Resulting product CoSe₂@NGN-20, was washed and saved for further uses. Other compositions were prepared using similar procedure after changing the amount of NGN as 5, 10 and 15 as CoSe₂@NGN-5, CoSe₂@NGN-10 and CoSe₂@NGN-15 respectively.

2.3 Cell fabrication and measurement

The detailed of counter electrode (CE) and DSSC fabrication processes, material characterization, and electrochemical measurement could be found in the Supporting Information.

The CoSe₂@NGN nanocomposite was prepared using reduction and post calcination method as shown in figure-1.

The FTIR spectra of the nanocomposites illustrate in figure 2(a) and the peaks at 1567 cm⁻¹ and 1647 cm⁻¹ assigned to the C=C and C=N bonds. Other peaks at 1334, 1402, and 1054 cm⁻¹ peak are assigned to the C-O, C–N, and C–O–C stretching, respectively (Ahamad et al., 2020a; Ahamad et al., 2019). While the peaks in the region of 3170-3382 cm⁻¹ are corresponding to N−H, -NH₂, and O−H bonds, respectively and the FTIR peak at 587 cm⁻¹ support the bond Co-Se. The thermal stability of the nanocomposites was determine using TGA analysis and the results were illustrated in the figure 2(b). The TGA outcomes revealed that as the amount of the NGN was increased from 5–20% the thermal stability of the nanocomposites was decreased and the reduced weight was found to be 49.02%, 41.64%, 38.43% and 34.88% corresponding to CoSe₂@NGN-5, CoSe₂@NGN-10, CoSe₂@NGN-15 and CoSe₂@NGN-20 respectively at 800 ^oC (Ahamad and Alshehri, 2013; Naushad et al., 2015). The purity and the crystalline nature of the nanocomposites were also determine using XRD, as shown in figure 2(c), The diffraction peaks at 2θ = 30.78, 34.52, 35.96, 40.38, 47.72, 50.23, 53.48, 56.95 and 63.29 can be assigned to the (101), (111), (120), (210), (211), (002), (031), (131) and (122) planes are assigned to the orthorhombic CoSe₂ (PDF-53–0449). The doping of the nitrogen atoms into to the graphene and growing the CoSe₂ nanoparticles into the NGN matrix was further determine using Raman spectra. As shown in figure 2(d), two main Raman peaks were observed at 1354 cm⁻¹ and 1592 cm⁻¹ known as D and G bands, respectively. The G band assigned to the sp² hybridized C=C bonds, whereas the D band assigned to the sp³ hybridized C-C bond (Ahamad et al., 2020c; Ahamad et al., 2020d; Alhokbany et al., 2020). The intensity of these two peaks increased with increasing the contents of NGN in to the nanocomposites. Other peaks at 163.46, 469.23 and 670.21 cm⁻¹ assigned to the CoSe₂ nanoparticles. The defect density of carbon is proportional to the value of I_D/I_G and found to be 1.24 in the case of CoSe₂@NGN-15.

The results indicated that the doping of N atoms and the existence of sp³ C-C and C-N bonds enhanced the disordered of graphene lattice. Which lead the electron transfer and catalytic efficiency for I₃⁻ reduction in DSSC. The microstructure and the morphology of the fabricated electrode materials were determine using SEM and TEM techniques. As shown in figure 3(a), the SEM image of the CoSe₂@NGN-15 nanocomposite show the porous structure and grown the nanoparticles in the NGN matrix. The enlarged pattern of the SEM image is shown in figure 3(b) and the results revealed that revealed that the spherical shaped CoSe₂ nanoparticles with the dimeter range of 20-50 nm are well dispersed into the NGN matrix. These results support that the fabricated electrode material contains hetrostructure which being conducive to the exposure the active sites at the surface of the catalyst to reduce the I₃⁻. To deep understand the microstructural of CoSe₂@NGN-15, TEM analysis was used. As shown in figure 3(c), CoSe₂ nanoparticles with an average size of ∼38.9 nm are uniformly embedded in the NGN matrix.

The HRTEM image as shown in figure 3(d), displayed inter-planar spacing of 0.29 nm, and 0.19 nm in the high-resolution TEM (HRETM) images are indexed to the (101), and (211) oriented facets of CoSe₂ nanoparticles. The inserted figure od selected area electron diffraction show the polycrystalline nature of the CoSe₂ nanoparticles. To porosity of the nanocomposites were further characterized using the nitrogen adsorption-desorption isotherm and the curves were illustrated in figure 4(a).

It was noticed that all the nanocomposites show type-IV hysteresis loops and demonstrating the mesoporous structure (Alshehri et al., 2017; Alshehri et al., 2016; Vinu et al., 2018). In the case of the CoSe₂@NGN-15, the hysteresis loops were observed from 0.40 to 0.99 and the specific surface area was found to be 421.0 m²/g, while for CoSe₂@NGN-5, CoSe₂@NGN-10, CoSe₂@NGN-20 the surface area was found to be 440.2, 436.4 and 414.12 m²/g respectively. These results demonstrate that the surface area of the nanocomposites were increased with increasing the contents of NGN into the electrode materials. Figure 4(b) show the pore size dimeter was observed about in the range of 20-67 nm in the case of all the nanocomposites. The large surface area and nanoscale pore size of the CoSe₂@NGN based electrode materials not only support the additional catalytic sites but also enhance the electron transfer during the I₃⁻ reduction. The elemental composition and the valance state of the elements present in the nanocomposite as monitored by XPS analysis, as shown in figure 5(a), the XPS spectra of CoSe₂@NGN-15 show the presence of C, N, Co, Se and O into the nanocomposite. As shown in figure 5(b), the C 1s peak was deconvoluted into four peaks and cantered at at 284.68, 285.71, 286.90 and 287.78 eV and assigned to the C-C, C-N, C=N, and O=C-O function groups presence into the NGN matrix.

The N1s spectra of the nanocomposites was split into three peaks and show the binding energy at into 398.24, 400.36, and 401.43 eV, corresponding to pyridinic, pyrrolic/pyridonic, and graphitic nitrogen functional groups respectively as shown in figure 5(c) (Ahamad et al., 2020b; Khalaf et al., 2020). The XPS peak of Co 2p was deconvoluted into four characteristic peaks as shown in figure 5(d), two of them are the main peaks and the binding energy cantered at 778.71 and 793.89 eV corresponding to the Co 2p_3/2 and Co 2p_1/2, respectively, and other two peaks were observed at binding energy 780.23 and 796.91 eV are assigned to the satellite peaks of Co 2p_3/2 and Co2 p_1/2 respectively. Figure 5(e), shows the XPS spectrum of Se 3d and the main peak was split into two peaks and cantered at 54.74 and 55.83 eV and assigned to Se 3d_3/2 and Se 3d_5/2 respectively (Liu et al., 2016). The XPS results shows that the O atoms also present into the matrix and the O 1 s spectrum was deconvoluted into binding energies of 530.44, and 531.88 eV and assigned to the presence of C-O and Se-O bonds respectively.

The DSSC was fabricated as sandwich structure using the the N719 dye-loaded TiO ₂ as a photo-anode, an iodine solution (I₃⁻/I⁻) as an electrolyte, and CoSe₂@NGN (or Pt) as a counter electrode. The current density voltage curve (J−V) of the fabricated DSSCs using CoSe₂@NGN-5, CoSe₂@NGN-10, CoSe₂@NGN-15, and CoSe₂@NGN-20 and Pt under 100 mW/cm² AM 1.5 G are illustrated in figure 6(a). The values of photovoltaic factors including short circuit current density (J_sc), open circuit voltage (V_oc), filling factor (FF) and maximum power (P_max) are summarized in table-1. It was observed that DSSC fabricated using CoSe₂@NGN-15, show excellent photovoltaic performance than other electrode materials prepared in this study. The short-circuit photocurrent (J_sc) of DSSC fabricated using CoSe₂@NGN-15 CE was found to be 15.40 mA/cm², higher than that of CoSe₂@NGN-5 (13.58 mA/cm²), CoSe₂@NGN-10 (14.21 mA/cm²), and CoSe₂@NGN-20 (15.10 mA/cm²), even outperforming that of Pt CEs (14.56 mA/cm²). The higher value of the J_sc is help to boost the reduction of I₃⁻ and dye regeneration (Niu et al., 2018; Wang, Q. et al., 2019). The open-circuit voltage (V_oc), fill factor (FF) and the PCE was found to be 0.74 V, 66.45% and 7.65% respectively for CoSe₂@NGN-15, while these values were obtained about to 0.74, 66.10%, 7.19% with Pt counter electrode. The excellent performance of CoSe₂@NGN-15 can be attributed due to the synergetic effect between CoSe₂ nanoparticles and NGN matrix, because the NGN matrix has excellent conductivity and the uniformly dispersed CoSe₂ nanoparticles provide excellent catalytic activity for I₃⁻ reduction.

Table 1: PCE values and relevant parameters of the different CEs

Counter Electrode	J_sc (mA cm⁻²)	V_oc (V)	FF (%)	PCE (%)
CoSe₂@NGN-5	13.58	0.731	66.73	6.62
CoSe₂@NGN-10	14.21	0.755	67.77	7.27
CoSe₂@NGN-15	15.40	0.745	66.66	7.65
CoSe₂@NGN-20	15.10	0.757	64.32	7.35
Pt	14.56	0.746	66.10	7.19

Moreover, the CoSe₂@NGN-15 nanocomposite has proper distribution as well as as greater the specific surface area of the counter electrode, and the higher the catalytic activity, and the better the photovoltaic performance of DSSC. On the other hand, the nanocomposites CoSe₂@NGN-5 and CoSe₂@NGN-10 show the DSSC performance lower than that of Pt. Based on the above results the proposed photovoltaic mechanism of the CoSe₂@NGN-5 CE is illustrated in Figure 7.

The relationship between the photoelectric conversion efficiency of the fabricated DSSC with the counter electrode was further carried out using CV, EIS and Tafel plots. As shown in figure 8(a), the cyclic voltammetry cure of the DSSC fabricated using CoSe₂@NGN-5, CoSe₂@NGN-10, CoSe₂@NGN-15, and CoSe₂@NGN-20 and Pt show the peaks due to the redox reaction of I₃⁻ as: I₃⁻ + 2e⁻→ 3I⁻ (i) and 3I₂ + 2e⁻ → 2I₃⁻ (ii). It was noticed that the the current density (J) and the potential (ΔE_pp) difference between the two peaks are important factors for comparing the catalytic activity of different CE materials. It was observed that the CE based on CoSe₂@NGN-15 nanocomposite show higher current density and lower peaks difference than these of Pt, indicating that CoSe₂@NGN-15 has superior catalytic ability than Pt for I₃⁻reduction (Kavan et al., 2011; Swami et al., 2015). The stability experiment was carried out using CV cycles as shown in figure 8(b), and the outcomes revealed that after 50 cycles on 50 mV/sec scan rate, the current density, peak positions and E_PP value is substantially unchanged, indicating CoSe₂@NGN-15 having excellent electrochemical stability.

The electrocatalytic activity of the CoSe₂@NGN-5, CoSe₂@NGN-10, CoSe₂@NGN-15, and CoSe₂@NGN-20 and Pt electrode were further determine using the Tafel polarization curves asillustrated in figure 8(c). All the Tafel polarization plots were divided into three zones, first the polarization zone occurs due to the electrochemical reaction and noticed at low over potential (|V| <120 mV), in the second zone is sharp slope is and it is Tafel zone, in which, the current density(J_o) is changed and noticed at moderate over-potentials (120 mV < |V| < 400 mV), third is the limiting diffusion zone, which depend on the transport of ions and occurs at high over-potential (|V|> 400 mV), and used to determine the limiting diffusion current density (J_lim). The value of of J_o and J_lim related to the catalytic activity of the counter electrode. As shown in figure 8(c), it has been noticed that CoSe₂@NGN-15 has a higher value of J_o as compared to Pt based CE, resulting shown higher catalytic activity towards I₃⁻ reduction, and the higher J_lim value of CoSe ₂@NGN-15, indicate that CoSe₂@NGN-15 based CE has a faster ion diffusion rate than standard Pt CE (Roy-Mayhew et al., 2010). The electrochemical impedance spectroscopy (EIS) measurements of the DSSC fabricated using CoSe₂@NGN-5, CoSe₂@NGN-10, CoSe₂@NGN-15, and CoSe₂@NGN-20 and Pt based CE is illustrated in figure 8(d). The EIS results used to determine various resistances, charge-transfer between the interface of electrode/electrolyte and the catalytic efficiency of the counter electrode.

The EIS Nyquist plots, show three semicircles, the R_s is represent to resistance between the FTO and CE materials, the R_ct−1 is representing to the charge transfer resistance between the electrolyte and CEs and the R_ct−2 represents the electron transfer resistance between the TiO₂/electrolyte and the dye. It was noticed that in all the Nyquist plots the value of R_ct−2 is unchanged and almost similar, these results may have been due to the use of similar type photoanaode materials. While the value of R_s and R_ct−1 was changed. The results reveal that CoSe₂@NGN-15 show almost similar value of Rs to the Pt and support that these is a good connection between the FTO glass and the electrode materials. While the R_ct−1 value of CoSe₂@NGN-15 was found to be lower, than that of other electrodes even lower than that of Pt based CE. On the other hand, it was noticed that the the CoSe₂@NGN-15 nanocomposite show lower value of Nernst diffusion impedance (Z_w) than the Pt base CE for diffusion of I⁻/I₃⁻ redox couple within the electrolyte (Kavan et al., 2011; Swami et al., 2015). This may be due to the existence of active site to contact with the electrolyte without any hindrances and resulting show excellent photoelectric conversion efficiency in the fabricated DSSC.

Sustainability has been the focus of researcher vision; therefore, we have fabricated novel counter electrode materials for DSSC using CoSe₂ nanoparticles embedded into NGN. The fabricated nanocomposites CoSe₂@NGN were characterized using several analytical techniques. The experimental results show that the CoSe₂@NGN electrode has excellent catalytic activity. Among them, the DSSC assembled by CoSe₂@NGN-15 obtains 7.65% PCE, which is higher than that of the DSSC assembled with Pt electrode (7.19%). The influence of different film thickness on the photovoltaic performance of DSSC was studied and discussed in depth. The excellent performance of CoSe₂@NGN-15 is attributed due to the synergetic effect of CoSe₂ nanoparticles and N-doped graphene matrix, because the N-doped graphene exhibit excellent conductivity and uniformly dispersed CoSe₂ which boost the catalytic activity of the nanocomposites. The preparation of this new type of non-Pt material provides a new method for DSSCs counter electrode research and promotes its industrialization process to utilised the sustainable solar energy for the benefit of humans.

6. Acknowledgement

The authors thanks to Researchers Supporting Project number (RSP-2021/6), King Saud University, Riyadh, Saudi Arabia.

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Reviews received at journal
11 Jan, 2022
Reviewers invited by journal
08 Jan, 2022
Editor assigned by journal
23 Dec, 2021
First submitted to journal
22 Dec, 2021

You are reading this latest preprint version

CoSe₂@N-Doped Graphene Nanocomposite High-Efficiency Counter Electrode For Dye-Sensitized Solar Cells

Status:

Version 1

Abstract

Figures

Introduction

Experimental

2.1 Materials

2.2 Preparation of CoSe₂@NGN

2.3 Cell fabrication and measurement

Results And Discussion

Photovoltaic Performance

Electrochemical Performance Of Ce Materials

Conclusion

Declarations

6. Acknowledgement

References

Supplementary Files

Status:

Version 1

CoSe2@N-Doped Graphene Nanocomposite High-Efficiency Counter Electrode For Dye-Sensitized Solar Cells

Status:

Version 1

Abstract

Figures

Introduction

Experimental

2.1 Materials

2.2 Preparation of CoSe2@NGN

2.3 Cell fabrication and measurement

Results And Discussion

Photovoltaic Performance

Electrochemical Performance Of Ce Materials

Conclusion

Declarations

6. Acknowledgement

References

Supplementary Files

Status:

Version 1

CoSe₂@N-Doped Graphene Nanocomposite High-Efficiency Counter Electrode For Dye-Sensitized Solar Cells

2.2 Preparation of CoSe₂@NGN