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Li, H.; Yang, Z. Production of 2D Bismuthene. Encyclopedia. Available online: https://encyclopedia.pub/entry/46323 (accessed on 26 July 2024).
Li H, Yang Z. Production of 2D Bismuthene. Encyclopedia. Available at: https://encyclopedia.pub/entry/46323. Accessed July 26, 2024.
Li, Haoran, Zhibin Yang. "Production of 2D Bismuthene" Encyclopedia, https://encyclopedia.pub/entry/46323 (accessed July 26, 2024).
Li, H., & Yang, Z. (2023, July 03). Production of 2D Bismuthene. In Encyclopedia. https://encyclopedia.pub/entry/46323
Li, Haoran and Zhibin Yang. "Production of 2D Bismuthene." Encyclopedia. Web. 03 July, 2023.
Production of 2D Bismuthene
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This entry is adapted from the peer-reviewed paper 10.3390/app13126885

Bismuthene exhibits layer-dependent direct bandgaps, high carrier mobility, and topological insulator properties because of its unique structure and ultrathin nature, distinguishing it as a promising candidate for photonic applications. Particularly, its outstanding stability in air makes bismuthene more advantageous than phosphorene for practical applications. Effective fabrication methods to realize high quality bismuthene are the key to realizing devices with outstanding performance. It is well known that top-down and bottom-up methods are the two main strategies for synthesizing 2D materials.

2D materials chemical vapor deposition top-down large-area growth pulsed laser deposition

1. Introduction

In recent years, two-dimensional (2D) elemental materials from group-VA (P, As, Sb, and Bi) have ignited increasing research interest in various of applications, including electronics, optoelectronics, energy related applications, spintronics, and biomedicine [1][2][3][4][5][6][7]. Unlike graphene, with its semi-metallic characteristics, 2D group-VA materials normally exhibit semiconducting characteristic with considerable bandgaps, making them favorable for electronic applications [8]. Among group-VA materials, phosphorene is the first, and up until now, the most-studied 2D candidate, attracting significant interest for use in many research fields, thanks to its high carrier mobility over 10,000 cm2V−1s−1, its tunable direct bandgaps from 0.3 eV (bulk) to 2.0 eV (monolayer), and its unique in-plane anisotropic properties [9][10][11]. However, phosphorene suffers from low stability when exposed to air, which should be optimized before considering the development of practical applications [12][13]. Recently, other 2D group-VA materials (As, Sb, Bi), namely arsenene, antimonene, and bismuthene have come into the spotlight due to their intrinsic wide band gaps, high carrier mobility, and good stability, which avert the main drawbacks of phosphorene [4].
As the last and heaviest element in group VA, bulk bismuth (Bi) exhibits a semi-metallic feature, with a small effective mass, a large mean free path, remarkable light-matter interaction, and low carrier density [14][15][16]. A previous study showed that Bi exhibits strong intrinsic spin-orbit coupling and conductive surface states, making it desirable for spintronic applications [14]. In general, when the thickness is thinner than the Fermi wavelength, Bi will undergo a transition from semimetal to semiconductor due to the quantum confinement effect [17][18]. Moreover, 2D Bi has been reported to possess unique surface states and band structures, demonstrating layer-dependent topological properties [17][19]. In 2017, Reis et al. successfully synthesized a graphene-like bismuthene film on top of a SiC substrate, showing a topological energy gap of 0.8 eV, which renewed the research interest in atomically thin Bi [20]. Since bismuthene exhibits a small band gap, a large nonlinear refraction index, and ultrahigh carrier mobility, the material is favorable for photonic applications such as broadband photodetectors [19][21][22], mode-locked lasers [18][23][24], and all-optical switching [25][26]. For example, Tang et al. demonstrated an ultrasensitive terahertz photodetector based on 2D bismuth. The strong photoresponse observed was attributed to the asymmetric scattering of topological surface states, which was stimulated by the localized surface plasmon-induced terahertz field. Furthermore, 2D bismuthene shows a large specific surface area, a hexagonal lattice structure, and high stability in air, making it suitable for photocatalytic applications [27][28][29]. In addition, the saturable absorption ability of bismuthene makes it applicable in Q-switched lasers. Recent study has reported a universal photo-redox catalyst based on few-layer bismuthene nanosheets, demonstrating arrested catalytic activity in an organic transformation under various reaction conditions [28].

2. Production of 2D Bismuthene

Effective fabrication methods to realize high quality bismuthene are the key to realizing devices with outstanding performance. It is well known that top-down and bottom-up methods are the two main strategies for synthesizing 2D materials. In general, the top-down strategy for fabricating 2D bismuth includes mechanical exfoliation, liquid-phase exfoliation, chemical exfoliation, etc. [30][31]. Common bottom-up fabrication methods include chemical vapor deposition (CVD) [22], pulsed laser deposition (PLD) [17], molecular beam epitaxy (MBE) [32], and electron beam (e-beam) evaporation [33]. In this section, several methods for the production of bismuthene will be described, and the advantages and drawbacks of each are also discussed.

2.1. Top-Down Approach

With the assistance of the proper chemical solvents and sonication processes, the interlayer vdWs force of bulk Bi can be broken to obtain 2D Bi nanosheets [24]. Bulk bismuth was ground into power using isopropyl alcohol. Subsequently, the bismuth isopropyl solution was subjected to both bath and probe sonication for 10 h, respectively. Next, 2D bismuthene was obtained after the centrifugation process. It should be noted that the type of chemical solvent used is of great significance for the efficient production of bismuthene nanosheets. The exfoliation efficiency can be optimized when the solvent’s surface tension component ratios are comparable to those of bismuthene [34].
As an efficient and low-cost method, liquid exfoliation can fabricate high-quality Bi with high efficiency and yield [35]. The strong interaction between bulk Bi and a suitable solution (such as isopropyl alcohol) leads to the dispersion of the bismuth nanosheets in the solvent [36]. In 2019, Huang et al. exfoliated Bi nanosheets from Bi powder in an ethanol solution using sonication-assisted liquid exfoliation [35]. Few-layer Bi was prepared after 1 h of sonication at 950 W and centrifugation at 500 rpm. According to the atomic force microscope (AFM) image, monolayer bismuth nanosheets were successfully fabricated. However, owing to defects in the exfoliation process, the exfoliated layers are not of high quality. In addition, the lateral size of the as-produced nanosheets ranges from the nm scale to the multiple μm scale. The optimization of the exfoliation process in order to better control the size of the obtained samples should be addressed in the future.
In addition to the liquid exfoliation process, 2D Bi can also be fabricated by the electrochemical exfoliation method due to its high chemical durability and the low cost of bulk metallic Bi [37][38]. Thanks to the advantages of short production time, moderate fabrication conditions, and high yield, the electrochemical exfoliation method provides a favorable platform for the mass production of 2D nanosheets. When bismuthene is prepared using a standard electrochemical exfoliation method based on a DC voltage apparatus, bulk Bi works as the cathode, and platinum foil works as the anode. During the fabrication process, both are soaked in the proper organic solution. The exerted bias facilitates the insertion of cations between the molecular layers, which can effectively increase the interlayer spacing. In 2019, 2D Bi, with a lattice fringe of 0.23 nm, was successfully exfoliated using a rapid electrochemical cathodic exfoliation method, resulting in Bi nanosheets with a large reactive surface area, beneficial for electrocatalytic performance [38]. Thanks to the significant field influence and the capacity to precisely tune the voltage, electrochemical exfoliation is an effective method to produce 2D Bi with good crystallinity and high yield [37][39]. However, owing to the introduction of organic solvents, the residues of the solution restrict the quality of the exfoliated samples.

2.2. Bottom-Up Approach

In addition to the top-down methods, a series of bottom-up methods have also been utilized in the fabrication of 2D Bi layers. CVD is one the most widely used bottom-up methods used to synthesis 2D materials. In 2020, Zhou et al. successfully grew 2D Bi films on both rigid (SiO2/Si) and flexible (polyimide) substrates using CVD. Bi powder in a silica boat is placed in the heating zone of the furnace. Using the flow of N2 gas in the tube, the Bi film will formed on the substrates, which are located downstream of the system [40]. The size and thickness of the CVD-grown 2D bismuth nanosheets can be controlled by tuning the key preparation parameters, such as reaction atmosphere, gas flow rate, processing temperature, and reaction time [41]. Over the last 5 years, Hu et al. have synthesized high quality Bi nanoflakes on Cu foil substrate using CVD. By introducing an h-BN top layer, the structural transformation of 2D Bi is effectively restricted. After removing the h-BN layer by mechanical exfoliation, 2D Bi nanoflakes show extraordinary thermal stability evidenced by the phenomenon of its ability to resist oxidization after annealing at 500 °C for 10 min. It is also significant that the obtained 2D Bi nanoflakes could be applied in electrochemical CO2 reduction reactions, retaining high crystallinity beyond 15 h.
PLD is one of the most effective physical methods to synthesize large-scale 2D materials and heterostructures [42]. During the PLD procedure, focused laser pulses strike the bulk target, and the generated energetic plasma plume is collected on a pre-heated substrate. In contrast to CVD, the processing temperature of 2D materials using PLD is usually relatively low. In addition, PLD exhibits the advantages of a high growth rate, better controllability of the film, and stoichiometric growth. In 2019, the group grew high crystallinity centimeter-scale Bi layers using PLD [17]. The 2D Bi(111) and Bi(110) thin films can be both produced by tuning the processing temperature at 100 °C and room temperature, respectively The thickness of Bi(111) and Bi(110) can be precisely controlled by the number of laser pulses. Meanwhile, the large scale and uniform surface give PLD-grown bismuthene great potential for developing practical device applications [42].
MBE is another commonly used bottom-up method to synthesis high quality 2D films and nanostructures [43][44]. The preparation process is realized in an ultrahigh vacuum chamber, which could prevent contamination by impurities. MBE is suitable for producing large-scale films with a consistent thickness, and can be processed with several types of in situ characterization equipment, such as reflection high-energy electron diffraction (RHEED) systems, to monitor the fabrication process, which can rarely be achieved in other bottom-up methods. In order to synthesis bismuthene, bulk Bi is heated to sublimation in an MBE system, forming a 2D Bi thin film on the substrates [32][45]. By tuning the substrate temperature, different phases of bismuthene are synthesized [46]. For example, Nagao et al. have grown multiple-layer 2D Bi films on Si(111) substrate using MBE [47]. The ultrathin Bi films with a (012)-oriented phase were generated above the wetting layer. This bismuth structure, discovered for the first time, is similar to the teratoid phase of BP.
Besides PLD and MBE, e-beam evaporation is also feasible for the synthesis of 2D-layered Bi [33][48]. Table 1 shows the comparison of the growth conditions and the material quality of 2D materials obtained using different fabrication techniques. In summary, the bottom-up synthesis of bismuthene is a significant complement to the top-down methods. The successful realization of wafer-scale few- and mono-layer bismuth films builds a solid foundation for the future development of high-performance photonic applications based on bismuthene.
Table 1. Comparison of techniques to fabricate bismuthene.
Size Throughput Thickness Homogeneity Fabrication Rate Processing Temperature Refs
Liquid exfoliation 1–10 μm High Moderate Moderate RT [24]
[35]
Electrochemical exfoliation 1–10 μm High Moderate Moderate RT [38]
CVD Over 1 cm High Very High Slow High [40]
PLD Over 1 cm High High Fast Moderate [17]
MBE   High High Slow High [46]

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