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Hydrogen 2023, 4 198 reported elsewhere and did not carry any additional information [12,18,42,67,68]. Figure 4a shows highly dispersed and well-shaped TNR with length ca. 50–70 nm. Figure 4b shows rGO nanosheets that are folded at the edges and Pd nanoparticles of an average particle size of 2–5 nm, which are uniformly distributed over the rGO sheets with no agglomerates. After blending rGO with TNRs, Pd structural features are not clearly seen due to very low loading amounts (4 wt.%). Figure 4c shows the hybrid nano-composites in which TiO2 nanorods are clearly interconnected by the rGO sheets. This type of hybrid structure is highly beneficial for vectorial charge transfer from TiO2 to catalytically active metal sites for proton reduction and enhancing the photocatalytic efficiency [69]. The intimate contacts in Hydrogen 2023, 4, FOR PEER REVIEW 7 the heterojunction of three components, i.e., TNRs, rGO and Pd particles are clearly noted in Figure 4d. Figure 2. (a) FTIR spectrum of pristine rGO. (b) Raman spectra of pristine rGO, Pd /rGO and Hydrogen 2023, 4, FOR PEER REVIEWFigure 2. (a) FTIR spectrum of pristine rGO. (b) Raman spectra of pristine rGO, Pd11/rGO4 4and8 Pd /rGO -TNR. 1 Pd1/rG4O4-TNR. Figure 3 shows the C 1s XPS spectra for Pd1/rGO4−TNR. After deconvolution, it is clearly evident that the C1s spectrum contains seven peaks at 282.7, 284.5, 285, 286.5, 288, 289 and 290.9 eV, corresponding to the carbidic carbon (C≡C)2− as well as carbon bonded to Pd, sp2 carbon (C=C), sp3 carbon (C-C, C-H), hydroxyl carbon (C-OH, C-O-C), carbonyl carbon (C=O), carboxyl carbon (O-C=O) and π→π* satellites, respectively [65]. A peak area ratio of more than five between sp2 carbon and hydroxyl carbon indicates the pres- ence of graphene in its reduced state [66]. Palladium is found to present as Pd and PdO. Given the fact that Pd is reduced very easily under X-rays, it is most likely that it is mainly present as PdO. This leads to the main reason behind the induction period ob- served during the photoreforming reaction where PdO was converted into Pd metal to reach steady state rates. We did not present Ti3d and O1s spectra, as they were similar to what has been reported elsewhere and did not carry any additional information [12,18,42,67,68]. Figure 4a shows highly dispersed and well-shaped TNR with length ca. 50–70 nm. Figure 4b shows rGO nanosheets that are folded at the edges and Pd nano- particles of an average particle size of 2–5 nm, which are uniformly distributed over the rGO sheets with no agglomerates. After blending rGO with TNRs, Pd structural features are not clearly seen due to very low loading amounts (4 wt.%). Figure 4c shows the hy- FiguFreig3u.reX3P.SXCPS1sC(1as)(an) adnXdPXSPSPdP3dd3d(b(b))ssppeeccttra of Pd1//rGrGOO4−T−NTRN. TRh.eTinhseetininse(ta)inis(a)reiscalreeds(ca)led brid nano-composites in which TiO2 nanorods are clearly interconnected by the rGO (a) totoclcelaeralrylysshhoowXPS C1s peaks wiitthaarreelalatitviveleylylolwowereirnitnentesnitsyi.ty. sheets. This type of hybrid structure is highly beneficial for vectorial charge transfer from TiO2 to catalytically active metal sites for proton reduction and enhancing the pho- tocatalytic efficiency [69]. The intimate contacts in the heterojunction of three compo- nents, i.e., TNRs, rGO and Pd particles are clearly noted in Figure 4d. 14PDF Image | Enhanced Photoreforming of Oxygenates
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