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Nanomaterials 2022, 12, 3528 Nanomaterials 2022, 12, 6 of 13 Figure 4. Zeta potentials of two kinds of MWCNTs plotted against ball milling time. Insert photo Figure 4. Zeta potentials of two kinds of MWCNTs plotted against ball milling time. Insert photo shows suspensions of two kinds of ultra-short CNTs, which were prepared by 24 h ball milling shows suspensions of two kinds of ultra-short CNTs, which were prepared by 24 h ball milling treatment and acid pickling. These two suspensions were left standing for 100 days. treatment and acid pickling. These two suspensions were left standing for 100 days. 3.2. KCl Enrichment Inside Ultra-Short CNTs 3.2. KCl Enrichment inside Ultra-Short CNTs Our previous work [42] demonstrated the formation of highly concentrated ion ag- Our previous work [42] demonstrated the formation of highly concentrated ion aggre- gregations inside MWCNTs soaked in dilute salt solutions. However, the CNT-filling ef- gations inside MWCNTs soaked in dilute salt solutions. However, the CNT-filling efficiency ficiency was always low when the MWCNTs were long, i.e., tens of micrometers in was always low when the MWCNTs were long, i.e., tens of micrometers in length. Ion 6 of 14 Nanomaterials 2022, 12, image of a CNT soaked in 0.14 M KCl shown in Figure 5a. Except for the tube mouth, most the tube mouth, most of the long CNT was empty, although some salt aggregations were length. Ion aggregations at the mouths of long CNTs were easily observed, as demon- aggregations at the mouths of long CNTs were easily observed, as demonstrated by the strated by the high-angle annular dark field scanning transmission electron microscopy high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM) (HAADF-STEM) image of a CNT soaked in 0.14 M KCl shown in Figure 5a. Except for of the long CNT was empty, although some salt aggregations were observed in the middle observed in the middle of the long CNT (Figure 5b). of the long CNT (Figure 5b). Accordingly, we reasoned that the unobstructed ultra-short CNTs would show a reduced incidence of blockage by salt aggregation (Figure 5a and Figure S2) or other blocking materials (Figure 3a–c). Figure 5c shows an HAADF-STEM image of an ul- tra-short MWCNT that was soaked in 0.14 M KCl solution. Salt aggregations filled near- ly the entire ultra-short CNT. Elemental mappings showing the distribution of the ele- ments C, O, K and Cl of the salt aggregation in the ultra-short CNT are also illustrated. The signal for C was the same shape as the CNT. The signals for K and Cl were high-intensity and located in the middle of the range of the C signal, and their widths were similar to the inner diameter of the CNT. Furthermore, the O signal, mainly from water inside the tube and functional groups on the tube, had a dispersive width equal to that of the C signal and was a little higher in the middle. Thus, the EDS mapping of the ultra-short CNT demonstrated that the tube was filled with high-concentration KCl so- lution. Figure 5. (a) A high-angle annular dark field scanning transmission electron microscopy Figure 5. (a) A high-angle annular dark field scanning transmission electron microscopy (HAADF- 7 of 14 (HAADF-STEM) image of a KCl aggregation at the mouth of a long CNT. (b) An HAADF-STEM STEM) image of a KCl aggregation at the mouth of a long CNT. (b) An HAADF-STEM image showing image showing the mid-section of a long CNT. (c) An HAADF-STEM image of a KCl aggregation the mid-section of a long CNT. (c) An HAADF-STEM image of a KCl aggregation inside an ultra-short inside an ultra-short CNT and the corresponding EDS mappings. (d) EDS results for the aggrega- CNT and the corresponding EDS mappings. (d) EDS results for the aggregation in (c) (the Mo signal tion in (c) (the Mo signal comes from the Mo sample grid). (e) K/O atomic ratios (blue points) of 16 coamggersegfraotmiontsheinMsidoesa1m6pralendgormid)u.l(trea)-sKh/oOrtaCtNomTsicarnadtiotshe(bKlu/eOproaitniots)offt1h6eaogugtrseidgeatisonlustionnside (dashed line). (f) Filling length/total length ratios for these 16 ultra-short CNTs. 16 random ultra-short CNTs and the K/O ratios of the outside solution (dashed line). (f) Filling length/total length ratios for these 16 ultra-short CNTs. Figure 5d shows the EDS results of the aggregations demonstrating that C, O, K and Cl were present. Furthermore, 16 salt aggregations in ultra-short CNTs were ran- domly selected and their K/O atomic ratios are shown in Figure 5e, indicating that the concentrations of these salt aggregations might be at least 1–2 orders of magnitude higher than that in the solution outside the CNTs. The K/C mass ratios of the aggrega- tions were also tens of times higher than that in the solution outside the CNTs (see morePDF Image | Ion Enrichment inside Ultra-Short Carbon Nanotubes
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