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Reusable GaN Nanowire Mediated Photocatalytic Reaction

The development of homogeneous photoredox catalysts in radical coupling reactions has been truly phenomenal, and the generation of new carbon–carbon bonds in an atom economical manner is a continuous pursuit in synthetic organic chemistry. This enables the production of many pharmaceutical compounds and bio-active molecules. The use of photoredox catalysts has quickly realized the huge potential in organic synthesis to afford facile coupling reactions enabled by photo-energy. Many excellent examples have been seen in the literature, including couplings of carbonyl-a-radicals [1] and ketyl radicals (e.g. the Pinacol Coupling Reaction, PCR) [2]. However, despite many successful applications of photoredox catalysts in radical coupling reactions, with some exceptions the scarce and expensive ruthenium (Ru) and iridium (Ir)-based homogeneous catalysts are predominantly used, which are difficult to isolate and recycle at the end of the reactions.

Over the past few years, engineering of group III-nitride semiconductor nano-structures and their applications as photocatalysts are well explored. Compared to common semiconductor catalysts [3] such as CdS, TiO2 and polymeric carbon nitride (PCN), the gallium nitride (GaN) semiconductor shows extraordinary stability [4, 5].

Figure 1. Scheme for radical coupling of carbonyl reactions carried out under blacklight irradiation using GaN nanowire (NW) as a reusable photoredox catalyst [5].
By carefully repositioning of the conduction band (CB) energy level and the valence band (VB) energy level of GaN NWs with doping, the desired direction of the electron flow can be established upon light irradiation on the GaN NWs. The photo-excited electron (e-) can efficiently be donated from the semiconductor to the reactant (H2O, N2, or CO2, respectively) to form the desired product (H2, NH3, or CO/hydrocarbon, respectively). At the same time, the photo-excited hole (h+) can be readily neutralized by many common sacrificial reagents. Inspired by these studies, we contemplate the possibility of using those unique characters of GaN NWs to design a more suitable and highly recyclable photoredox catalyst for radical coupling reactions under a light.
The surface energy band bending significantly influences the electronic properties of semiconductors [6]. Upon light irradiation, the excited e- in the CB of the semiconductor tends to migrate to the potential energy well. In contrast, the h+ on the VB tends to migrate to high potential energy (high ground). These surface band properties inhibit carrier recombination and give rise to unique reactivities. By doping the NW with a tetravalent element (e.g. silicon, germanium, etc.) as the n-type dopant, the surface energy band of GaN bends upward to give n-GaN NWs. Upon light irradiation [6], the excited e-in the CB tends to migrate to the internal region of the NW instead of the surface, while the h+ in the VB tends to migrate to the surface instead of the internal region of the NW. Such doping prohibits edonation to the reactant and enhances the neutralization of h+ by the sacrificial reagent (Figure 2A). On the other hand, by using a divalent element (e.g., magnesium) as the p-type dopant, the surface energy band of the corresponding NW bends downwards (p-GaN NW).
Figure 2.  (A) Surface energy band bending of the GaN NW. (B) EPR identification of band bending [5].

The photoexcited efor the p-GaN NWs will therefore tend to aggregate on the NW surface, making the donation of eto the reactant easier, while the h+ tends to migrate to the internal region of the NWs and inhibits the consumption of the sacrificial reagent (Figure 2A right). To characterize these electronic properties, electron paramagnetic resonance (EPR) spectra were recorded for the as-synthesized intrinsic- (i-), n-, and p-GaN NWs; they were irradiated under 365 nm light (Figure 2B) for 1 hour [7]. Since both Ga3+ and N3- do not possess unpaired electron, the ground state of GaN is diamagnetic. Therefore, the observed EPR signal should exclusively come from photoexcited electrons (EPR spectra of i-, n-, and p-GaN NWs in the dark were silent). It can be observed from the EPR spectra that both n- and p-GaN NWs show stronger EPR signals than i-GaN NWs. This is because the photoexcited eand h+ are more prone towards recombination in i-GaN NWs are due to less influential band bending.
In concluding, they report a photo-pinacol coupling reaction catalyzed by GaN nanowires under ambient light at room temperature with methanol as a solvent and sacrificial reagent. By simply tuning the dopant, the GaN nanowire shows significantly enhanced electronic properties. The catalyst showed excellent stability, reusability and functional tolerance. All reactions could be accomplished with a single piece of nanowire on Si-wafer. 

References

  1. D. A. Nicewicz and D. W. C. MacMillan, Science, 322, 77 (2008).

  2. L. J. Rono et al., J. Am. Chem. Soc., 135, 17735 (2013).

  3. A. Caron et al., ACS Catal., 9, 9458 (2019).

  4. M. G. Kibria et al., Adv. Mater. 28, 8388 (2016).

  5. M. Liu et al., Chem. Sci. 11, 7864 (2020).

  6. M. G. Kibria et al., Nat. Commun. 5, 3825 (2014).

  7. M. Foussekis, Band Bending in GaN, Master dissertation, Virginia Commonwealth University, Richmond, Virginia (2009). 

Blog Written By

Dr. Y. Sasikumar

School of Materials Science & Engineering

Tianjin University of Technology

Tianjin, China

Editors

Dr. A. S. Ganeshraja

Dr. K. Rajkumar

Dr. K. Chandrasekar

Reviewers

Dr. K. Vaithinathan

Dr. S. Thirumurugan

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