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Nanomaterials 2021, 11, 1017 5 of 12 Nanomaterials 2021, 11, x FOR PEER REVIEW 5 of 12 FFiiggurree11..XXRRDDpaptatettrenrsnosfo: f(:a)(aP)dP/Cd/o3COo43@OM4@WMCWNTC;N(bT);P(bd)/MPdW/CMNWT;C(Nc)TC; o(c3O) C4 @oM3OW4 C@NMTW; (CdN) fT-; (d) Mf-WMWCNCTNsT; s(e; )(eJ)CJPCDPSDfSilfieloefoPfdP;d(;f)(fJ)CJPCDPSDoSfoCf oC3oO4O. . 34 The successful synthesis of the Pd/Co O @MWCNT composite was confirmed via The successful synthesis of the Pd/Co3O44@MWCNT composite was confirmed via TEM and SEM, as shown in Figure 2. Figure 2a presents the surface morphology of the TEM and SEM, as shown in Figure 2. Figure 2a presents the surface morphology of the compositecomprisingCoO nanoparticlesuniformlycoatedonthesurfaceofthefunc- composite comprising Co3O3 4 4nanoparticles uniformly coated on the surface of the func- tionalized MWCNTs. The diameter of the MWCNTs varied from 50 to 80 nm. The surfaces tionalized MWCNTs. The diameter of the MWCNTs varied from 50 to 80 nm. The surfaces of the acid-treated MWCNTs were mostly uniform without any defects, indicative of a of the acid-treated MWCNTs were mostly uniform without any defects, indicative of a homogeneouslayerofCoO particlesontheMWCNTs,whichaffordedhighuniformity homogeneous layer of Co33O44particles on the MWCNTs, which afforded high uniformity without agglomeration of the particles. Figure 2b,c illustrates that the Pd/Co O @MWCNT 34 without agglomeration of the particles. Figure 2b,c illustrates that the Pd/Co3O4@MWCNT composite was obtained with a relatively homogeneous distribution of the particles. How- composite was obtained with a relatively homogeneous distribution of the particles. How- ever,somePdaggregatesandCoO nanoparticleswerestillpresentonthesurfaceofthe 34 ever, some Pd aggregates and Co3O4 nanoparticles were still present on the surface of the MWCNTs, which could hinder the catalytic activity of the composite owing to the limited MWCNTs, which could hinder the catalytic activity of the composite owing to the limited surface area. This observation is attributed to de-adhesion of the Pd nanoparticles from the surface area. This observation is attributed to de-adhesion of the Pd nanoparticles from Co3O4@MWCNT composite because of weak metal bonding interactions among the parti- the Co3O4@MWCNT composite because of weak metal bonding interactions among the cles [4,25]. Figure 2d-h presents elemental mapping of the prepared Pd/Co3O4@MWCNT particles [4,25]. Figure 2d‒h presents elemental mapping of the prepared as a means of reconfirming the distribution of each element in the obtained composite. The Pd/Co3O4@MWCNT as a means of reconfirming the distribution of each element in the estimated particle size of Pd and Co3O4 could be obtained from TEM images. The sizes of obtained composite. The estimated particle size of Pd and Co3O4 could be obtained from Pd nanoparticles varied from 4.52 nm to 9.09 nm, and the Co3O4 nanoparticles varied from TEM images. The sizes of Pd nanoparticles varied from 4.52 nm to 9.09 nm, and the Co3O4 9.53 nm to 16.21 nm. The mean sizes of Pd particles and Co3O4 particles were estimated as nanoparticles varied from 9.53 nm to 16.21 nm. The mean sizes of Pd particles and Co3O4 7.62 nm and 13.18 nm from the TEM pictures, which are shown in Figure 2i,j. Furthermore, particles were estimated as 7.62 nm and 13.18 nm from the TEM pictures, which are shown the particle size distribution of Pd/Co3O4 in Figure 2k was highly corresponding to the in Figure 2i,j. Furthermore, the particle size distribution of Pd/Co3O4 in Figure 2k was size distribution of the nanoparticles in the individual components. It is clear that there highly corresponding to the size distribution of the nanoparticles in the individual com- were distinguishable size differences of Pd particles and Co3O4 particles in the obtained ponents. It is clear that there were distinguishable size differences of Pd particles and Pd/Co3O4@MWCNT composite. Co3O4 particles in the obtained Pd/Co3O4@MWCNT composite. The high concentration of oxygen vacancies could facilitate oxygen adsorption and covalent metal oxide–nanocarbon bonding and enable improved electron transfer across the interface. The specific surface area of Pd/Co3O4@MWCNT was 190.89 m2 g−1, as obtained from the BET data presented in Figure 3. Besides, the BET specific surface area results of MWCNTs, Co3O4@MWCNT, and Pd/MWCNT were 89.8 m2 g−1, 110.2 m2 g−1, 132.1 m2 g−1, respectively. The large specific surface area of the synthesized composite facilitated the adsorption and transport of O2 and H2O during the ORR.PDF Image | Effect of Co3O4 Nanoparticles on Improving Catalytic Behavior
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