Developing a highly efficient water-splitting photocatalyst for hydrogen production under visible light is urgent. In this study, β-SiC nanowire photocatalysts loaded with 0.01–0.1 wt. % nickel were prepared. Their microstructure and hydrogen production activity were studied. The catalyst with 0.05 wt. % nickel and a sacrificial agent Na2S–Na2SO3 shows the highest hydrogen production rate of 375.4 µmol g−1 h−1 since the loaded nickel prohibits the recombination of photogenerated electron–hole pairs in the system, which enhances the photocatalytic activity.

Hydrogen (H2) is widely considered as an ideal energy carrier to replace other energy sources and fulfill our needs sustainably in the future owing to its highest gravimetric energy density and zero emission. Among many hydrogen production methods, photocatalytic water splitting is the most promising way for converting solar energy into hydrogen energy.1,2 Since the work by Fujishima and Honda,3 extensive studies have been conducted for photoelectrochemical H2 production by photocatalysts.4–6 

To achieve a high photocatalytic hydrogen production rate, it is essential to develop high-performance photocatalysts. Semiconductor materials are a main group of photocatalysts due to their superior charge separation efficiency and high reactive radicals.7 At present, semiconductors such as TiO2,8,9 g-C3N4,10,11 Cds,12 MoS2,13,14 biomass,15,16 MOF,17 ZIF,18 perovskite materials,19 ZnO,20 MXene,21 and cerium22 are widely used as photocatalysts. However, most of those catalysts are active only under ultraviolet light, which accounts for a small part of sunlight, limiting their practical applications. Thus, semiconductor photocatalysts with a suitable bandgap that is active under visible light are of great interest and regarded as an ideal technology for the sustainable development of the hydrogen energy industry.

As a well-known third-generation semiconductor, silicon carbide (SiC) is becoming one of the hotspots in the field of photocatalysis research due to its high thermal stability, chemical inertness, oxidation resistance, and mechanical strength.23,24 SiC is frequently adopted as a support in photocatalysts,25–28 and several SiC polytypes with suitable band edge potentials, such as 4H–SiC, 6H–SiC, and 3C–SiC, exhibit water splitting ability under light irradiation.29 In addition, the suitable bandgap makes β-SiC a very attractive and suitable candidate for photocatalytic hydrogen conversion applications.30 

However, SiC powders exhibit weak photocatalytic activity, and various strategies have been developed to improve the photoactivity. Among them, morphology engineering has been considered as one of the most feasible methods.31,32 Solar water splitting can occur over SiC only if SiC is tailored into nano-sized particles, nanowires, or nanorods. Particularly, nanowires with a high specific surface area enrich active sites to enhance the thermodynamic driving force for H2 evolution reaction.31 Moreover, cocatalyst modification is essential in photocatalytic systems, which can accelerate the separation and transportation of photogenerated charge and significantly accelerate the surface reactions on heterogeneous photocatalysts. Besides traditional noble metallic cocatalysts (e.g., Au, Ag, Pt, and Ni),33–35 nickel-based catalysts, such as NiO,36 Ni2P,37 NiS,38 and metallic Ni,39–41 are also favorable cocatalyst candidates due to their high abundance, low cost, easy preparation, chemical stability, and high efficiency.

Herein, we highlight porous β-SiC nanowire sponge photocatalysts with crosslinked structures and cost-effective nickel cocatalysts, which can inhibit the undesired combination of photogenerated electron–hole pairs. The achieved photocatalytic H2 evolution rate of β-SiC nanowire sponge was as high as 375.4 µmol g−1 h−1, which is ascribed to the synergistic effect of the β-SiC nanowire structure and nickel species in preventing photoinduced electron–hole recombination and boosting the hydrogen evolution reaction.

High-purity argon (Ar, purity ≥99.999%) was purchased from the Guangming Research Institute of Chemical Industry, China. Ni(NO3)2 · 6H2O, Na2S, Na2SO3 were obtained from Shanghai Aladdin Bio-chem Technology Co. Ltd., China. Commercial melamine foam (Dongguan Yueyang Group Co. Ltd., Guangdong, China) with high porosity (∼96%) and polycarbosilane (PCS; Suzhou Ceramic Fibers Co. Ltd., China) powder, with a number-average molecular weight of around 1400, were used in this study.

Highly flexible carbon foam is prepared by direct carbonization of commercial melamine foam. The melamine foam is placed into the vacuum tube furnace and then heated to 900 °C at a ramping rate of 10 °C/min for carbon foam preparation. Then, the carbon foam is immersed in a nickel nitrate solution (0.01, 0.02, 0.05, and 0.1 wt. %; the corresponding samples are marked as 1#, 2#, 3#, and 4#, respectively) for 30 s and air-dried at room temperature. Afterward, the sample is heated at a rate of 5 °C min−1 from room temperature to 500 °C for 2 h. After that, the carbon foam is reduced with H2 at 500 °C for 1 h, resulting in the formation of uniformly distributed nickel nanoparticles. Polycarbosilane dissolved in heptane (20 wt. %) was deposited on/inside the carbon foam; then the coated carbon foam was air-dried at room temperature and pyrolyzed at 1300 °C at a heating rate as 5 °C min−1 in vacuum for 2 h to form β-SiC nanowires with 3D interconnected networks [Fig. 1]. The raw product was collected after the furnace was cooled down to room temperature and then purified by oxygen calcination and acid treatment (etching in an HNO3 + HF solution: nHNO3/nHF = 2:1).

FIG. 1.

Schematic diagram of fabrication procedures of β-SiC nanowire sponge.

FIG. 1.

Schematic diagram of fabrication procedures of β-SiC nanowire sponge.

Close modal

The electrochemistry tests are carried out using a CHI660D electrochemical workstation (Shanghai Chenhua, China). The as-prepared β-SiC electrode with conductive glass, carbon rod, and Ag/AgCl (saturated KCl) electrode serve as the working electrode, counter electrode, and reference electrode, respectively. Linear sweep voltammetry (LSV) is performed at a scan rate of 5 mV/s between 0 and -0.4 V vs RHE to obtain the polarization curves. Cyclic voltammetry (CV) is carried out between 0.1 and 0.2 V vs RHE at the same scan rate from 10 to 100 mV/s. Electrochemical impedance spectroscopy (EIS) from 0.01 Hz to 1 MHz is conducted with an alternating current voltage of 5 mV.

The photocatalytic performance is determined by a H2 photocatalytic hydrogen evolution system (LabSolar, Beijing Perfectlight) with a 300 W xenon lamp (PLS-SXE300, Beijing Perfectlight, China) and a UV cut-off filter (λ > 420 nm). The hydrogen concentration is measured using a gas chromatograph (GC-1300, TCD). Photocatalytic hydrogen production occurs in a 100 ml enclosed quartz refractory glass reactor with 100 mg β-SiC nanowire sponge. Na2S–Na2SO3 is used as a sacrificial agent, and the activity for H2 evolution is normalized by per unit weight.

The crystalline structure of SiC nanowires is characterized by x-ray diffractometry (XRD, Philips X′ Pert) with Cu–Kα radiation. The morphology is examined using a field emission scanning electron microscope (FESEM, Hitachi-4800) and transmission electron microscope (TEM, JEOL-1011). The ultraviolet-visible diffuse reflectance spectrum is measured using a spectrophotometer (UV-3600, Shimadzu). The elemental states are analyzed by x-ray photoelectron spectroscopy (XPS, Thermo Scientific ESCALAB™ 250Xi).

The crystalline structure and hydrogen production efficiency of β-SiC nanowire loading with different amounts of nickel are systematically studied, and the results are shown in Fig. 2. With the increase in the nickel content, the hydrogen production efficiencies increase remarkably and reach the maximum when the nickel content is 0.05 mol/l (sample 3#), showing a H2 yield of 11.1 µl after 3 h reaction. The absorption edge of the sample red-shifts with increasing nickel content (in the range of 0.01–0.05 wt. %), indicating that nickel can promote charge separation, consequently leading to a higher hydrogen production amount [Fig. 2(a)]. However, excessive nickel is not beneficial to photoactivities. The H2-production rate of sample 4# (0.1 wt. % nickel) decreases abruptly since excessive nickel covers the active sites on SiC nanowires and blocks the light [Fig. 2(b)]. Therefore, 0.05 wt. % nickel is optimum for photocatalytic H2 production in the present case. Moreover, it is observed that samples after acid etching [Fig. 2(c)] exhibit ∼5 times higher yield of H2-production than the sample without etching. This can be explained as follows: as shown in XRD patterns [Fig. 2(d)], sample 3# is composed of 3C–SiC (β-SiC) and SiO2. After etching, diffraction peaks of SiO2 disappear. Except for the peaks of β-SiC, no other crystalline phases such as silica, carbon, or other impurities have been detected, indicating that the employed etching process successfully removes the SiO2 in the nanowire and the remaining β-SiC nanowire exhibits high catalytic activity [Fig. 2(d)].

FIG. 2.

Comparison of photocatalytic H2 volume before (a) and after (c) acid etching with different nickel contents (1#: 0.01 wt. %, 2#: 0.02 wt. %, 3#:0.05 wt. %, and 4#:0.1 wt. %); (b) UV-visible absorption spectrum of β-SiC nanowires after acid etching; (d) XRD pattern of β-SiC nanowires before (3#) and after acid etching (3-2#).

FIG. 2.

Comparison of photocatalytic H2 volume before (a) and after (c) acid etching with different nickel contents (1#: 0.01 wt. %, 2#: 0.02 wt. %, 3#:0.05 wt. %, and 4#:0.1 wt. %); (b) UV-visible absorption spectrum of β-SiC nanowires after acid etching; (d) XRD pattern of β-SiC nanowires before (3#) and after acid etching (3-2#).

Close modal

The SEM and TEM images, accompanied by the corresponding fast Fourier transform [FFT, inset in Fig. 3(c)] pattern, of the β-SiC nanowires after acid etching are shown in Fig. 3. Most of these nanowires are curved [Fig. 3(a)] with a smooth surface and good crystallinity [Figs. 3(b) and 3(c)]. Lattice fringes with a distance of 0.25 nm [Fig. 3(d)] in the HRTEM images are attributed to the (111) planes of the β-SiC crystal [Fig. 3(e)].32 The element mapping spectrum of β-SiC nanowires in [Fig. 3(f)] indicates that C and Si are the main components and a certain amount of Ni also exists.

FIG. 3.

Morphological and structural characterizations of β-SiC nanowire sponge. (a) and (b) surface SEM images; (c) TEM together with the corresponding FFT patterns [inset in (c)]; (d) and (e) HRTEM and (f) elemental mapping images.

FIG. 3.

Morphological and structural characterizations of β-SiC nanowire sponge. (a) and (b) surface SEM images; (c) TEM together with the corresponding FFT patterns [inset in (c)]; (d) and (e) HRTEM and (f) elemental mapping images.

Close modal

The valence states of elements in SiC nanowires were determined by XPS. The coexistence of C, Si, and Ni in the nanowires is confirmed [Fig. 4(a)]. Two C 1s signals with binding energies of 284.05 (C–C) and 285.6 (C–Si) are detected [Fig. 4(b)]. Two peaks with binding energies of 98.6 and 101.75 eV in the Si 2p region can be assigned to the covalent bonding of Si–C and Si–O, respectively [Fig. 4(c)].42 For the Ni spectrum [Fig. 4(d)], two peaks at 856.25 and 874.15 eV assigned to Ni 2p3/2 and Ni 2p1/2, respectively, were also observed, indicating the presence of Ni.

FIG. 4.

High-resolution XPS spectra of the β-SiC nanowires with the nickel cocatalyst: (a) full spectrum; (b) C1s, (c) Si 2p, and (d) Ni 2p.

FIG. 4.

High-resolution XPS spectra of the β-SiC nanowires with the nickel cocatalyst: (a) full spectrum; (b) C1s, (c) Si 2p, and (d) Ni 2p.

Close modal

β-SiC nanowires with the sacrificial agent Na2S–Na2SO3 exhibit higher H2 evolution performance with a H2 production rate of 375.4 µmol g−1 h−1 than the one without the Na2S–Na2SO3 system, as shown in Fig. 5(a). As is well-known, sulfur vacancies could serve as an active center to improve the photocatalytic activity for hydrogen evolution with Na2S–Na2SO3 as the sacrificial agent due to their special redox capacity, which was beneficial for fast hole consumption,43,44 thus restraining the hole-induced photo-corrosion and enhancing the H2-evolution rate, as shown in Fig. 5(a). To further demonstrate the stability of the β-SiC nanowire photocatalyst for hydrogen generation, the cycle test is carried out under identical conditions as the one shown in Fig. 5(b). The β-SiC nanowire photocatalyst can maintain a relatively stable and high H2 production rate. After four cycles, the H2 production rate does not exhibit a significant decrease [Fig. 5(b)]. Moreover, β-SiC nanowires exhibit excellent structure stability as no obvious changes in morphology and XRD patterns (crystal structure) can be observed [Figs. 5(c) and 5(d)]. The existence of C and Si in the nanowires is shown in Fig. 5(e), and the sample has two peaks in the Raman spectrum, as shown in Fig. 5(f) after the photocatalysis; the two peaks present at ∼801 and 990 cm−1 correspond accurately to the TO and LO of β-SiC, respectively. It is proved that the silicon carbide nanowires are stable after the photocatalysis for 40 h over the four-cycle operation.

FIG. 5.

(a) H2 production activity of the β-SiC nanowires with and without the Na2S/NaSO3 sacrifice reagent; (b) cycle activities of samples under visible-light irradiation; (c) SEM, (d) XRD, (e) XPS, and (f) Raman patterns after the photocatalysis for 40 h over the four-cycle operation.

FIG. 5.

(a) H2 production activity of the β-SiC nanowires with and without the Na2S/NaSO3 sacrifice reagent; (b) cycle activities of samples under visible-light irradiation; (c) SEM, (d) XRD, (e) XPS, and (f) Raman patterns after the photocatalysis for 40 h over the four-cycle operation.

Close modal

Finally, a comparison between the H2 evolution activity for the β-SiC nanowire catalyst in this work and those (carried out on other photocatalysts) reported in the literature3–8 is shown in Table I. The H2 evolution activity values in the present work of nickel-loaded β-SiC nanowires is lower than those of CdS and MoS2 (metal sulfide-based catalysts), but they are at a comparable level of the reported values of Au–Ni, COF, TiO2/carbon dots, and USTC-8. It is important to note that it is easy to recover the nanowire catalyst at the end of the reaction, so the nickel-loaded β-SiC nanowires is a promising catalyst for photocatalytic H2 production by water splitting.

TABLE I.

Summary of H2 evolution activity of photocatalysts in recent years.

PhotocatalystsActivity (μmol g−1 h−1)Reference
Nickel-loaded 375.4 This work 
β-SiC nanowires   
Au–Ni 246 45  
CdS@g‐C3N4 4390 46  
COF 233 47  
MoS2 4300 48  
TiO2/carbon dots 246 49  
USTC-8(In) 341.3 50  
PhotocatalystsActivity (μmol g−1 h−1)Reference
Nickel-loaded 375.4 This work 
β-SiC nanowires   
Au–Ni 246 45  
CdS@g‐C3N4 4390 46  
COF 233 47  
MoS2 4300 48  
TiO2/carbon dots 246 49  
USTC-8(In) 341.3 50  
Figure 6(a) shows the UV–vis absorption spectra of the samples. The optical absorption edge of the SiC nanowire center is at ∼451 nm. In addition, the bandgap energies of all samples are determined by Kubelka–Munk transformation [Eq. (1)],51 
(αhν)1/2= A(hνEg),
(1)
where Eg is the bandgap energy, α is the absorption coefficient, A is a constant, ν is the light frequency, and h is Planck’s constant. Tauc’s plot of (αhν)1/2 vs photon energy was constructed and is shown in Fig. 6(b), and the bandgap energy of β-SiC nanowires is estimated to be 2.33 eV. The Mott–Schottky plot exhibits a positive slope [Fig. 6(c)], indicating that the SiC nanowires prepared in this work are n-type semiconductors. For an n-type semiconductor, the flat band potential (−0.20 eV) is very close to the conduction band (CB). The flat band potential (ESCE) of the present β-SiC nanowires (−1.10 eV) can be determined by extending the curve to construct the intersection point with the horizontal coordinate [as shown in Fig. 6(c)]. Then, we can propose that the conduction band edge position (ECB) of β-SiC nanowires should be at −1.30 V [Fig. 6(d)], while the valence band potential (EVB) should be at 1.03 V because the β-SiC nanowires have a bandgap (Eg) of 2.33 eV (−1.30 + 2.33 = 1.03 eV) [Eq. (2)],
EVB=ECB+Eg,
(2)
where EVB is the VB potential, ECB is the CB potential, and Eg is the semiconductor bandgap.
FIG. 6.

(a) UVvis diffusion absorption spectra; (b) Tauc’s plots; (c) the valence band potential and (d) schematic energy level diagram of β-SiC nanowires.

FIG. 6.

(a) UVvis diffusion absorption spectra; (b) Tauc’s plots; (c) the valence band potential and (d) schematic energy level diagram of β-SiC nanowires.

Close modal

Figure 7 shows the proposed photocatalytic hydrogen production mechanism of β-SiC nanowires with the nickel cocatalyst. The high H2-production activity of the β-SiC nanowires with the nickel cocatalyst under visible-light irradiation can be explained as follows:

FIG. 7.

Schematic of the proposed photocatalytic hydrogen production mechanism of β-SiC nanowires with the nickel cocatalyst.

FIG. 7.

Schematic of the proposed photocatalytic hydrogen production mechanism of β-SiC nanowires with the nickel cocatalyst.

Close modal
Under visible-light irradiation, electrons (e) are excited from the VB to CB to produce H2 [Eqs (3)(5)],
βSiC+hν=βSiC(e-+h+),
(3)
2h++H2O =1/2O2+2H+,
(4)
2H++2e-=H2.
(5)
Normally, these charge carriers quickly recombine, and only a fraction of electrons can effectively split H2O to produce H2 (E0 H+/H2 = 0 vs SHE, pH = 0). The conduction band minima are smaller than the H2O reduction potential (0 eV at pH 7), which is favorable for hydrogen evolution reaction. A more positive potential of the top of the valence band, i.e., stronger oxygen reduction capacity, is favorable for rapid oxidation of the sacrificial agent in hydrogen evolution reactions; thus, the holes in the VB of the catalyst can be consumed by the sacrificial agents (Na2S–Na2SO3), and the electron in the CB is captured by nickel. Therefore, the recombination of photogenerated electron–hole pairs (eh+) is inhibited, leading to the hole–electron separation, which effectively promotes the photogenerated electrons to participate in major reaction steps in photocatalytic water-splitting.

In summary, β-SiC nanowires for photocatalytic water splitting are successfully prepared by the carbothermic reduction method using polycarbosilane as the starting material. The β-SiC nanowire photocatalyst loaded with 0.5 wt. % nickel shows the best performance, which means the introduction of Ni as a cocatalyst increases the separation rate of photogenerated carriers and improves the photocatalytic performance of β-SiC nanowires. The β-SiC nanowires with the appropriate conduction band exhibit excellent hydrogen production performance with a hydrogen production rate of 375.4 µmol g−1 h−1, Thus, β-SiC nanowires can be regarded as a promising photocatalyst for photocatalytic H2 production by water splitting.

This work was financially supported by the Guangdong Major Project of Basic and Applied Basic Research (Grant No. 2021B0301030001), the Self-innovation Research Funding Project of Hanjiang Laboratory (Grant No. HJL202202A003), and the Key Research and Development Project of Hubei Province (Grant No. 2020BCA075).

The authors have no conflicts to disclose.

Ying Wang: Data curation (equal); Writing – original draft (equal). Shuai Yang: Writing – review & editing (equal). Xiang Li: Writing – review & editing (equal). Wei Huang: Supervision (equal); Writing – review & editing (equal). Zheng-fa He: Supervision (equal); Writing – review & editing (equal). Xian-liang Fu: Supervision (equal); Writing – review & editing (equal). Li Zhu: Funding acquisition (equal); Supervision (equal); Writing – review & editing (equal).

The data that support the findings of this study are available within the article.

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