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Nanomaterials 2022, 12, 3528 2.1. Preparation of Ultra-Short CNTs Raw long multi-walled carbon nanotubes (MWCNTs) with an average diameter of ~6 nm and an average length of 20 μm, and another kind of MWCNTs with diameters of 20–50 nm and an average length of 20 μm were purchased from Beijing DK Nano Tech- 98% H2SO4 and 70% HNO3 for 2 h to open the mouths. Then, the primary processed CNTs were ball milled with a planetary ball mill (QM-3SP04, 450 rpm) for 6–24 h. Finally, othfe9b8%allH-miSllOedasnhdor7t0C%NHTsNwOerefoarg2aihntsonoipceantetdheinmao3u:t1h(sv./Tvh)emni,xthuereporifm98a%ryHpr2SoOce4sasned 243 C70N%TsHwNeOre3 bfaolrl m40illmedinwtiothraemploavnetanraynobsacllamleililm(QpuMri-t3iSesP0(4re, s4i5d0uraplmca)tfaolrys6t–,2a4mho. rFpinhaolulys, tghreapbhailtle-,miniltlerdnashlodretfeCcNtsT,setwc.)e.reHeargea,insosnoincaictiaotneduisninag3a:110(v0/Wv)umltirxatusoreniocfc9le8a%neHraStO70 aknHdz7w0%asHcoNnOducfoterd4.0Amftienrtsourfefimcioenvtewnansohsincagl,eciemnptruifruitgieasti(ornes(i1d0u,0a0l0cagt,al3ysmt,inam) aonrdphvoaucs- 3 guruamphfitletr,aintitoenrn,tahlederefescutlst,inetgc.C).NHTesrew,esorenidcraiteiodnauts6i0ng°Caf1o0r02W4huilntrasvoancicuuclmeanoverenat.70kHz was conducted. After sufficient washing, centrifugation (10,000× g, 3 min) and vacuum fi2.l2tr.aCtNioTn,FtihlleinrgesEuxltpienrgimCeNntTss were dried at 60 ◦C for 24 h in a vacuum oven. nology Co., Ltd. These two kinds of MWCNTs were sonicated in a 3: 1 (v/v) mixture of KCl (purity ≥ 99.5 wt %), CaCl2 (purity ≥ 96.0 wt %) and FeCl3 (purity ≥ 97.0 wt %) 2.2. CNT Filling Experiments were purchased from Sinopharm Chemical Reagent Corporation (Shanghai, China). The KCl (purity ≥ 99.5 wt %), CaCl2 (purity ≥ 96.0 wt %) and FeCl3 (purity ≥ 97.0 wt %) ultra-short CNT samples (with diameters of 20–50 nm) treated by 24 h ball milling and were purchased from Sinopharm Chemical Reagent Corporation (Shanghai, China). The acid pickling were soaked in 0.14 mol/L (M) KCl, CaCl2 or PbCl2 solution for 20 min with ultra-short CNT samples (with diameters of 20–50 nm) treated by 24 h ball milling and sonication using a 100 W ultrasonic cleaner at 70 kHz. The ultra-short CNT samples were acid pickling were soaked in 0.14 mol/L (M) KCl, CaCl2 or PbCl2 solution for 20 min with removed from the solution and dried under an infrared lamp for 15–20 min. During the sonication using a 100 W ultrasonic cleaner at 70 kHz. The ultra-short CNT samples were drying process, the temperature was maintained in the range of 30–40 °C. removed from the solution and dried under an infrared lamp for 15–20 min. During the drying process, the temperature was maintained in the range of 30–40 ◦C. 2.3. Characterization The CNTs were characterized by TEM (FEI Tecnai G2 F20 TEM, 200 kV), and ele- 2.3. Characterization mental analysis was performed using EDS. Additionally, zeta potential (Malvern The CNTs were characterized by TEM (FEI Tecnai G2 F20 TEM, 200 kV), and elemen- Zetamaster, Malvern Instrument Ltd., Malvern, UK) measurement was used to deter- tal analysis was performed using EDS. Additionally, zeta potential (Malvern Zetamaster, mine the dispersibility of MWCNT nanofluids prepared using ball milling for different Malvern Instrument Ltd., Malvern, UK) measurement was used to determine the dis- times and acid pickling. The zeta potential of the MWCNT nanofluids was measured at persibility of MWCNT nanofluids prepared using ball milling for different times and acid pH 7.0. pickling. The zeta potential of the MWCNT nanofluids was measured at pH 7.0. 3. Results and Discussion 3.1. Shortening of CNTs 3.1. Shortening of CNTs Figure 1 shows the schematic of the fabrication of the ultra-short CNTs. The raw long Figure 1 shows the schematic of the fabrication of the ultra-short CNTs. The raw CNTs were shortened by ball milling and the blockages in the mid-section of CNTs were long CNTs were shortened by ball milling and the blockages in the mid-section of CNTs removed using the acid pickling method. were removed using the acid pickling method. 3 of 13 24 Figure 1. Schematic of the fabrication of ultra-short carbon nanotubes (CNTs) using ball milling Figure 1. Schematic of the fabrication of ultra-short carbon nanotubes (CNTs) using ball milling and and acid pickling methods. acid pickling methods. Ball miillilningghhasasbebeenenreproeprtoerdtetdo bteo abneefafnecteifvfecmtivetehomdeftohrogdrifnodringgriCndNiTnsgtoCsNhTorstetno tsheoirtelentghtheir[4l3e–n4g5t]h. T[4w3o–4k5i]n.dTswoof CkNinTdswofitChNsiTmsilwaritihnistimalileanrginthitsiablultedngiftfhersebnut tddiaimffertenrst wdiearmebetaelrlsmwilleerdeabnadllamciidllepdickalned.aFcigdupreic2kale,bdd.iFsipgluaryeth2ea,TbEdMispimlaaygethseofTtEhMeMimWaCgNesTsofwtihthe aMnWavCeNraTgsewdiiathmeatneraovfe~ra6gnemdibaemfoerteranodf a~f6tenrmtheb2e4fohrebalnldmiallfitnegr trheeat2m4enht.bFailglumreil2licn,dg strheoawtmtehnet.MFWiguCrNeT2sc,wdisthodwiamtheteMrsWinCNthTesrawnigthed20ia–m50etnemrsbineftohreerandgeaf2t0e–r5t0henm24bhefboarlel milling treatment. The 20–50 nm-wide MWCNTs were shorter and had more uniform lengths than the 6 nm-wide MWCNTs. These results indicate that the wider CNTs were more easily and efficiently shortened by ball milling.PDF Image | Ion Enrichment inside Ultra-Short Carbon Nanotubes
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