Electrochemical deposition of GaTe thin films for photoelectrochemical applications

doi:10.21203/rs.3.rs-2571661/v1

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Electrochemical deposition of GaTe thin films for photoelectrochemical applications

https://doi.org/10.21203/rs.3.rs-2571661/v1

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published 23 Jun, 2023

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GaTe thin films are electrochemically deposited on indium tin oxide for photoelectrochemical applications. The electrochemical deposition behavior of GaTe in acidic solution of HTeO₂⁺ with Ga³⁺ is studied with cyclic voltammetry combining with operando transmittance spectroscopy. Underpotential deposition of Ga on Te starts at potential of -0.35 V. The present of Ga³⁺ in the solution can strongly suppressed the formation of H₂Te. XPS analysis reveals that Ga-rich GaTe is deposited over a wide potential range. The photoelectrochemical performance of the thin films as photocathodes is strongly dependent on the deposition potential. The GaTe films deposited at -1.0 V produced the highest photocurrent of -0.06 mA cm^− 2 with good stability. Meanwhile the film deposited at -0.35 V shows improved performance during photoelectrochemical measurement, which can be ascribed to the increased GaTe content during photoelectrochemical measurements, as confirmed by XPS analysis.

Gallium Tellurium

Photoelectrochemical water splitting

Underpotential deposition

Layered material

Photoelectrochemical (PEC) water splitting as a promising routine for producing clean fuel of hydrogen using solar energy has attracted extended investigation [1]. Solar to hydrogen conversion efficiency of PEC cells is primarily determined by the photoelectrodes [2]. There are many intrinsic n-type semiconductors such as TiO₂ [3], BiVO₄ [4], WO₃ [5] and ZnO [6] that can be used as photoanodes. In contrast, only a few native p-type semiconductors can be used as photocathodes. Cu₂O as one of most representative photocathodes have been widely investigated [7, 8]. Recently, tellurium-based compound semiconductors such as CdTe [9] and ZnTe [10, 11] exhibiting potential application as photocathodes have attracted research interest.

Gallium tellurium (GaTe) is a layered III–VI van der Waals semiconductor, having high carrier mobility and long carrier lifetime [12, 13]. Undoped GaTe is a native p-type semiconductor with a direct bandgap around 1.7 eV and a high optical absorption coefficient [13]. GaTe has been investigated for potential applications in optoelectronic devices, such as radiation detectors [13], THz sources and sensors [14], solar cells [15, 16]. Recently, Li et. al. demonstrated the potential application of GaTe for PEC hydrogen production [17]. Photocatalytic degradation of methyl blue with GaTe nanowires and nanosheets was achieved by Tien et. al. [12]. However, the performance of the GaTe still does not satisfy photoelectrochemical applications, required further study.

Chemical vapor deposition (CVD) and physical vapor deposition (PVD) are usually used for synthesis of GaTe nanomaterials [12, 16, 17] that require high cost instruments and time consuming. Alternatively, electrochemical deposition is a promising and facile method to prepare semiconductor thin films due to its simplicity, low cost, ease of scale-up and environmental compatibility, which has been used for deposition of Te [18, 19], CdTe [9, 20], Bi₂Te₃ [21], ZnTe [22, 23] thin films. However, electrochemical deposition of GaTe has still rarely reported [24]. Therefore, the growth mechanism of GaTe thin film is not thoroughly understood. In this paper, we systematically study the electrochemical deposition behavior of Te and GaTe with cyclic voltammetry and operando transmittance spectroscopy. It is found out that the present of Ga³⁺ results in the growth of GaTe that strongly suppresses the formation of H₂Te. Coexistence of Ga and Te in the films deposited at a wide potential range from − 0.35 V to -1.0 V, revealing that GaTe can be deposited at potential as positive as -0.35 V. All the GaTe thin films can used as photocathodes and the one deposited at -1.0 V achieves the highest photocurrent of -0.06 mA cm^− 2.

Te and GaTe thin films were grown by electrochemical deposition that was carried out with the experimental setup sketched in Fig. 1. Briefly, a three-electrode cell was mounted at an optical microscope to monitor the growth of the Te and GaTe thin films with operando transmission spectroscopy. In the three-electrode cell, an indium tin oxide (ITO) covered glass, a Pt wire and an Ag/AgCl (saturated KCl) were used as the working electrode, counter electrode and reference electrode, respectively. Before deposition, the ITO substrates were clean in acetone, ethanol and water, sequentially. The electrode area of the ITO glass was confined to 0.2 cm² by a rubber O-ring. Solution was prepared by dissolution of tellurium oxide (TeO₂, 99.99%, Aladdin) into 0.1 M H₂SO₄. Then 0.05 M Ga(NO₃)₃ (99.99%, Aladdin) was added to the 0.1 M H₂SO₄ + 0.001 M TeO₂ solution to form 0.1 M H₂SO₄ + 0.001 M TeO₂ + 0.05 M Ga (NO₃)₃ solution. All the electrochemical experiments were conducted with an electrochemical workstation of CHI660D. Cyclic voltammetry (CV) was performed to study the deposition behavior of Te and GaTe. During CV measurements, the potential was scanned negatively from 0.3 V to -0.9 V (or -1.1 V) and then reversed to 0.7 V at a rate of 10 mV s^− 1. Transmission of white light emitted from a LED was simultaneously recorded with a Si diode detector (Thorlabs, PAD 100A-FS). After studying on the deposition behavior with CV, the thin films were deposited with chronoamperometry at different potentials of -0.35 V, -0.5 V, -0.6 V, -0.7 V, -0.8 V, -0.9 V and − 1.0 V.

Morphology of the thin films was imaged with a Hitachi S4800 scanning electron microscope (SEM). Relative diffuse reflectance spectra of the thin films in the range of 200 nm to 1000 nm were measured with a Shimadzu UV-3600 Plus UV–VIS-NIR spectrophotometer. X-ray photoelectron spectroscopy (XPS) was conducted with a Thermo Nexsa G2 equipped with the Al Ka (hn = 1486.60 eV) to characterize the surface composition of the thin films. All the XPS results were calibrated with the binding energy of C 1s photoelectrons of 284.8 eV.

Photoelectrochemical measurements were conducted with the same setup as the thin film preparation. 0.1 M H₂SO₄ was used as the electrolyte. During PEC measurements, the thin films deposited at different potentials were illuminated from backside with the white light LED (400-700nm, 10 mW cm^− 2).

3.1 Elecctrochemical deposition behavior of Te and GaTe

Figure 2a shows the cyclic voltammograms (CVs) of the ITO substrate in the solutions without and with Ga³⁺. The scanning direction of the CVs is instructed by the arrows. The simultaneously recorded transmission spectra are shown in Fig. 2b. HTeO₂⁺ formed by dissolution of TeO₂ in acidic solution is the electroactive species for deposition of Te and GaTe [18]. In the solution of 0.1 M H₂SO₄ + 0.001 M TeO₂, a cathodic peak at -0.36 V is observed, which is attributed to the reduction of HTeO₂⁺ to Te [19, 25], as described by Eq. (1):

$$\text{HTe}{\text{O}}_{2}^{+}+\text{3}{\text{H}}^{+}+\text{4}{\text{e}}^{-}\to \text{Te}+{\text{H}}_{2}\text{O }{ E}^{0}\text{=0.551 }{V}_{NHE} \left(1\right)$$

Upon the deposition of Te, the normalized transmittance decreases with the negatively scanning potential until the potential reaches − 0.71 V. There is another cathodic peak at around − 0.77 V observed, which is corresponding to the reduction of Te to H₂Te [19, 26], as described by Eq. (2):

$$\text{Te}+\text{2}{\text{H}}^{+}+\text{2}{\text{e}}^{-}\to {\text{H}}_{2}\text{Te }{ E}^{0}\text{=-0.47 }{V}_{NHE} \text{ }\left(2\right)$$

Consumption of the pre-deposited Te for producing gaseous H₂Te is proven by the slightly increased transmittance at around − 0.77 V. Dennison et. al. illustrated that the generated H₂Te would further react with HTeO₂⁺ to form a fine, densely packed Te film, as described by Eq. (3) [18]

$$\text{2}{\text{H}}_{2}\text{Te}+\text{HTe}{\text{O}}_{2}^{+}\to \text{3Te}+\text{2}{\text{H}}_{2}\text{O}+{\text{H}}^{+}\text{ }\left(3\right)$$

The Gibbs energy of reaction (3) is -500 kJ mol^− 1, pointing to a strong driving force for the spontaneous formation of the densely packed film [18], which is also indicated by the decreased transmittance. Hydrogen evolution occurred when the potential was more negative than − 0.8 V which is corresponding to the rapidly increase photocurrent.

At the reverse scan, the transmittance slightly increased at the potential range from − 0.7 V to -0.36 V, indicating the reduction of Te to H₂Te. At the potential range from − 0.36 V to -0.1 V, the transmittance decreased but without current detected, which probably could be attributed to decomposition of H₂Te to Te [26], following the Eq. (4):

$${\text{H}}_{2}\text{Te}\to \text{Te}+{\text{H}}_{2}\text{ }\text{ }\left(4\right)$$

One anodic peak at 0.45 V can be seen, which is due to the re-oxidation of Te to HTeO₂⁺ [18] and resulted in the rapidly increase transmittance.

As shown by the CV curve (in red) in Fig. 2a, the present of Ga³⁺ resulted in slightly positive shift of the first cathodic peak and higher cathodic current. Coexistence of Ga and Te of the film deposited at -0.35 V is evidenced by the X-ray photoelectron spectroscopic analysis (Fig. 4), indicating the co-deposition of Ga and Te. Similar behavior of deposition of CdTe over a wide potential range has also been observed by Dennison et. al [20]. In the range from − 0.8 V to -0.9 V, cathodic current significantly increases in the present of Ga³⁺ but the transmittance of the film just slightly decreases, indicating that the high cathodic current is corresponding to hydrogen evolution catalyzed by GaTe. At the reverse scan, the transmittance keeps increasing until the potential reached 0.35 V, demonstrating that the deposited Te would react with Ga³⁺ to form GaTe rather than reduced to H₂Te. The existence of the anodic peak at 0.45 V demonstrates that the deposited Te cannot be completely converted to GaTe even though the concentration of Ga³⁺ is excess. The coexistence of GaTe and Te does not affect the stability of the Te, as indicated by the unchanged position of the anodic peak.

As revealed by Fig. 2c, as the cathodic potential extends to -1.1 V, the transmittance rapidly decreases upon the formation of a thick Te film. The anodic peak at -0.36 V can be attributed to the oxidation of H₂Te to Te. This reaction makes the Te film become thicker rapidly, crack and peeling off finally. Differently, as indicated by the transmittance curve (in red), formation of GaTe upon the present of Ga³⁺, can efficiently suppress the formation of H₂Te even when the potential is extended to -1.1 V. The much higher cathodic current corresponding to hydrogen evolution also demonstrates the better catalytic performance of the GaTe than Te.

Chronoamperometry was conducted for deposition of thin films at different potentials. Figure 3a shows the j-t curves at different potentials and Fig. 3b shows the corresponding transmittance spectra. The corresponding top-view SEM images of the thin films are shown in Fig. 3c-Fig. 3i. Deposition currents at -0.35 V, -0.5 V, -0.6 V and − 0.7 V are comparable. However, the morphology of the thin films is very different. At -0.35V, granule morphology with many small nanoparticles is obtained (Fig. 3c). The granule morphology changes to feather-like structures at potential of -0.5 V (Fig. 3d) The thin films deposited at -0.6 V and − 0.7 V, there are many congregated flocs on the top. The thin films deposited at -0.9 V (Fig. 3h) exhibits a striped surface. The striped surface grows more homogeneously as the deposited potential increases negatively to -1.0 V (Fig. 2i). It is worth to notice that there is no change of the morphology for the sample after photoelectrochemical measurements (Fig. 2j).

3.2 Surface composition of the thin films

The surface compositions of the thin films deposited with different potentials were studied with XPS. The first column in Fig. 4 shows the high resolution XPS spectra of the Ga 3d of the as-prepared thin films deposited at -0.35 V, -0.9 V and − 1.0 V. According to Bondino, binding energy (BE) of Ga 3d of the defect-free GaTe is around 19 eV, but the BE peak would shift to lower energy for the Ga-rich GaTe_1 − x [27]. Therefore, the BE peak at 18.3 eV in Fig. 4a of the film deposited at -0.35 V is assigned to the Ga-rich GaTe. The growth GaTe is further demonstrated by the high resolution XPS spectra of Te 3d in Fig. 4d, where the BE peaks at 527.8 eV and 583.2 eV can be assigned to 3d_5/2 and 3d_3/2 of the Te²⁻, respectively [13]. In Fig. 4a, the BE peak at 17.7 eV is contributed by Ga⁰ [28], indicating the existence of metallic Ga and demonstrating the underpotential deposition of Ga at -0.35 V. Existence of Ga₂Te₃ phase is evidenced by the BE peak at 20.1 eV [4, 29]. In Fig. 4d, The BE peaks at 576.1 eV and 586.5 eV are corresponding to the 3d_5/2 and 3d_3/2 of Te⁴⁺, indicating the present of TeO₂ [13]. The existence of Te⁰ is evidenced by the BE peaks at round 574.0 eV and 584.3 eV [13]. The BE peaks at 576.5 eV and 586.8 eV can be assigned to TeO₃ [27]. Figure 4 (b) and (e) show the XPS of Ga 3d and Te 3d of the thin film deposited at -0.9 V. Similarly, GaTe, Ga, Ga₂Te₃, Ga₂O₃, Te, TeO₂ are found. In comparison with that deposited at -0.35 V, the relative intensity of Te²⁻ significantly increases, indicating the higher content of GaTe. Figure 4c shows the XPS of Ga 3d of the film deposited at -1.0 V, where the signal of Ga⁰ is highest. It is revealed that a certain amount of metallic Ga has been deposited at this potential.

The third and fourth column in Fig. 4 show the XPS spectra of the films after conducting PEC measurements. The chemical composition and phase have not strongly changed after PEC measurements, however, the content changed. Obviously, as shown by Fig. 4j, the signals of Te²⁻ strongly increases after PEC measurement, which reveals the content of GaTe increases. In contrast, as shown by Fig. 4h and Fig. 4k, after PEC measurements, the content of GaTe of the film deposited at -0.9 V slightly decreases, and the content of Ga increases.

3.3 Optical properties of the thin films

Figure 5. (a) shows the UV–vis-NIR diffuse absorption spectra for the thin films deposited with different potentials. Absorbance starts to decrease dramatically at around 700 nm. According to the Kubelka-Munk function:

$$(\alpha h\upsilon {)}^{n}\propto (hv-{E}_{g})$$

where α is absorption efficiency, hν is energy of the incident light, E_g is the band gap of the semiconductor, n is 0.5 for indirect semiconductors and is 2 for direct semiconductors, the band gap of the thin films can be deduced. Figure 5b shows the Tauc plots of the thin films derived from the diffuse reflectance UV-vis-NIR spectra via the Kubelka-Munk function. The E_g of the thin films is obtained to be 1.8 eV by the intercept the linear portion of the Tauc plots with the hv-axis.

3.4 Photoelectrochemical properties of the GaTe films

Figure 6a shows the open circuit potential (OCP) of the thin films responded to periodic illumination of white light. Firstly, under dark the OCP shifts negatively as the deposition potential changed from − 0.35 V to -1.0 V, which is helpful for increasing the energy of photo-generated electrons for photoelectrochemical (PEC) hydrogen evolution by moving the Fermi level negatively. On the other hand, OCP transient of the thin films is also strongly affected by the deposition potential. OCP of the thin films deposited with − 0.35 V and − 0.5 V did not respond to illumination at all. This indicates that the thin films deposited at these potentials have metal-like behavior initially. The OCP transient becomes obvious for the thin films deposited at -0.8 V, -0.9 V and − 1.0 V. The positive shift of the OCP demonstrates the thin films are p-type semiconductors. Figure 6b shows the linear sweep voltammograms (LSV) of the thin films. It is consistent with the OCP results that there is not photocurrent produced by the thin films deposited at -0.35 V and − 0.5 V. The thin films deposited at -1.0 V produced the highest photocurrent. Figure 6c shows the transient photocurrent of the thin films measured at -0.36 V_RHE. At the first 200 s after switching on illumination, the behavior of photocurrent with deposition potential is consequent with the OCP and LSV results. After that, it is interesting to observed that activation occurred and the photocurrent of all the thin film is rapidly increased. For example, photocurrent of the thin film deposited at -0.35 V is rapidly increased to -0.05 mA cm^− 2. By comparing the XPS results of the thin film before and after PEC measurements, it can be found out that the content of GaTe increased after PEC measurements. Thus, the activation process can be contributed to the increased content of GaTe at -0.36 V_RHE. The highest photocurrent of -0.06 mA cm^− 2 is achieved by the GaTe thin films deposited at -1.0 V, which has good photo-stability.

In this work, GaTe thin films were electrochemically deposited with acidic solution containing HTeO⁺ and Ga³⁺ as electroactive species. As revealed by the cyclic voltammetry combining with operando transmittance spectroscopy, the present of Ga³⁺ and growth of GaTe strongly suppressed the formation of H₂Te at the potential range from − 0.7 V to -1.1 V. On the other hand, underpotential deposition of Ga on Te occurred from the onset of deposition, as demonstrated by the coexistence of Ga and Te of the films deposited at different potentials. Photoelectrochemical measurements illustrated that the GaTe could be used as photocathodes for solar hydrogen production. The photoelectrochemical performance of the thin films was strongly determined by the deposition potential. Generally, the GaTe thin films deposited at -0.9 V and − 1.0 V generated high photocurrent. In-situ conversion of the underpotential deposited Ga to GaTe was attributed to the observed activation process during PEC measurements, as revealed by the XPS analysis.

Acknowledgements

This work was supported by the National Natural Science Foundation of China (No. 11504242); the Project of Guangdong Provincial Education (No. 2020KTSCX131); Research Fund of Guangdong-Hong Kong-Macao Joint Laboratory for Intelligent Micro-Nano Optoelectronic Technology (No. 2020B1212030010).

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No competing interests reported.

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You are reading this latest preprint version

Electrochemical deposition of GaTe thin films for photoelectrochemical applications

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Journal Publication

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Abstract

Figures

1. Introduction

2. Materials And Methods

3. Results And Discussion

3.1 Elecctrochemical deposition behavior of Te and GaTe

3.2 Surface composition of the thin films

3.3 Optical properties of the thin films

3.4 Photoelectrochemical properties of the GaTe films

4. Conclusions

Declarations

Acknowledgements

References

Additional Declarations

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Journal Publication

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