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Nanomaterials 2022, 12, 3788 6 of 19 Nanomaterials 2022, 12, x FOR PEER REVIEW 6 of 20 Figure 2. STEM images recorded for CoP drop‐casted on TEM grids from solutions obtained using Figure 2. STEM images recorded for CoP drop-casted on TEM grids from solutions obtained using the following solvents: (a) DMSO, (b) DMF, (c) CH3CN, (d) PhCN, (e) EtOH, and (f) THF. The insets the following solvents: (a) DMSO, (b) DMF, (c) CH3CN, (d) PhCN, (e) EtOH, and (f) THF. The insets are STEM and TEM images that provide additional information about the specimens. are STEM and TEM images that provide additional information about the specimens. The image recorded on the ZnP specimen obtained using DMSO as a solvent (Figure The image recorded on the ZnP specimen obtained using DMSO as a solvent (Figure 1a) 1a) shows irregular formations with micrometric lengths and widths, sprinkled with small shows irregular formations with micrometric lengths and widths, sprinkled with small particles sized between 30 and 180 nm. Irregular aggregates were also observed when the pasrotlivcelenstwsizasedDMbeFtw(Feigeunr3e01ba)n,dbu1t8t0henymw.erIerrmegixueldarwaigthgcreugbaotieds‐liwkersetrualcstouroebs.sWerhvieledtwhehen thlensogltvheanntdwwasidDthMoFf m(Foigstuoref t1hbe),idbuenttihfieydwsterurectmuriexsedwewreithmcicurboomidet-rlick,efostrrsuocmtuereosf.tWhehile thaerclehnitgetchtuarensdrewseidmtbhlionfgmcuobsotidofstheseiddeinmteifinesidonsstrwuecrtuerinesthweesruebmicromeetrtricicr,afnogres.Aomn‐e of thoetharecrhsitmeciltaurrietysbrestwemeebnlitnhgiscsupbeocimdsenthaensdedthiempernesviionuslwyedriesciunssthedesounbemcoincrsoismteedtrinictrhaenge. Anporethsenrcseimofilsamritayllbpeatrwtiecelenstohnistshpeescuimrfaecneaonfdththeeapssremviboluiessly, wdhisicleusaseddiffoenrenccoenwsiastsepdrion‐ the vided by the existence of crevices on the surface of some of the structures from the former presence of small particles on the surface of the assemblies, while a difference was provided sample. When applied from benzonitrile, the ZnP molecules organized as aggregates re‐ by the existence of crevices on the surface of some of the structures from the former sample. sembling cuboids and square plates (Figure 1c and inset). The measurements conducted When applied from benzonitrile, the ZnP molecules organized as aggregates resembling for several cuboids revealed widths between 1.38 and 1.7 μm and thicknesses in the 0.2– cuboids and square plates (Figure 1c and inset). The measurements conducted for several 0.44 μm range. It has been reported that complex porphyrin architectures comprise sim‐ cuboids revealed widths between 1.38 and 1.7 μm and thicknesses in the 0.2–0.44 μm range. pler ones, resulting from the side‐by‐side or face‐to‐face positioning of the molecules [50]. It has been reported that complex porphyrin architectures comprise simpler ones, resulting In the case of 3D aggregates—such as the ones observed for this specimen—these two from the side-by-side or face-to-face positioning of the molecules [50]. In the case of 3D types of assemblies, referred to as J‐type and H‐type arrangements, are both present [51]. aggregates—such as the ones observed for this specimen—these two types of assemblies, In the case of the ZnP samples obtained using the solvents with the lowest polarity, referred to as J-type and H-type arrangements, are both present [51]. the molecules no longer interacted to create irregular structures and cuboids but some In the case of the ZnP samples obtained using the solvents with the lowest polarity, very different aggregates instead (Figures 1d,e). Thus, when THF was employed as a sol‐ the molecules no longer interacted to create irregular structures and cuboids but some very vent, a discontinuous metalloporphyrin layer covered the carbon film of the TEM grid. different aggregates instead (Figure 1d,e). Thus, when THF was employed as a solvent, Ring‐shaped formations revealed the substrate and appeared brighter than the surround‐ a discontinuous metalloporphyrin layer covered the carbon film of the TEM grid. Ring- ing ZnP deposits, probably due to a higher concentration of molecules. The ring diameters shaped formations revealed the substrate and appeared brighter than the surrounding were in the 30–150 nm range. The inset in Figure 1d shows a magnified image of one of ZnP deposits, probably due to a higher concentration of molecules. The ring diameters the rings (ø = 150 nm). When ZnP was applied from DCM, the observed aggregates were were in the 30–150 nm range. The inset in Figure 1d shows a magnified image of one of the rings (ø = 150 nm). When ZnP was applied from DCM, the observed aggregates were island-shaped and displayed a tendency to organize into circular arrangements (Figure 1e) due to their helical growth.PDF Image | pH Water-Splitting Electrocatalytic Graphite Electrodes
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