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Molecules 2021, 26, x FOR PEER REVIEW 4 of 23 Molecules 2021, 26, 5276 4 of 22 The micrograph images of the transmission electron microscopy (TEM) analysis for the bamboo and the commercial CNF are shown in Figure 1a,b, respectively. The bamboo CNF and commercial CNF showed a similar TEM morphological pattern of irregular rod shape with network fibres. The bamboo CNF showed a well‐dispersed, rod‐like network with network fibres. The bamboo CNF showed a well-dispersed, rod-like network with no with no fibre bundles, while the commercial CNF still had some fibre bundles in its TEM fibre bundles, while the commercial CNF still had some fibre bundles in its TEM image. image. The bamboo CNF exhibited fibrous morphology, probably due to its precursor The bamboo CNF exhibited fibrous morphology, probably due to its precursor material m(patrerniat lfi(bpraer)e[2n2t,f2i3b]r.eA) [t2t2h,e23sa].mAetttihmees,athmeecotimme,etrhceiacloCmNmFesrhcoiawleCdNnFo rsehgouwlaerdfinborerleegnugltahr, fwibhriechlecnagntha,lswohbiechatctarinbualtseodbtoe aittstrsioburtceed(tcotitosns)o[u2r4c]e. C(comttomne)r[c2i4a]l.CNoFm(mCe-CrcNiaFl)CdNerFiv(eCd‐ CfrNomF)cdoetrtoivnedalfsroosmhocwotetodnirarlesgouslhaorwaned rirorueghulsaurrafnacdersowuigth suormfaecaegsgwreitghastoempaeratigcglerseg[2a4te]. pBarmticbloeos [C2N4]F. BhamdbaosomCaNlleFrhfiabdreassizmeatlhlearnficbormemsizeerctihalanCNcoFm,amsearncaialylsCeNdFu,sainsganpalrytiscelde usiszienganpaalrytsiicsl.eTshizeefiabnraelydsiaism.Tetheerfsibzreeisdoianmeefatecrtosriztheaistdoenterfmacitnoersththaetrdeeintefromrcienmesenthteabreilinty‐ fofrCceNmFenint caobmiliptyosoifteCsN[2F5]i.nSlciogmhtpmosoitrepsh[o2l5o]g.iScalilgdhitffmeroernpcheoslboegtiwcaelednifbfaemrebnoceosCbNetFwaenedn bcoambmoeorcCiaNl FCaNnFd’scopmhymsiecracliaplroCpNeFrt’iseps hcyousilcdalpprorobpaberlytiebsecdoueldtoprdoifbfaebrelyncbees dinuethteo sdoiuffrecre‐ eonfctehseinr rtahwe smouartceerioaflsthaenidr rtahweirmpartoedriuaclstiaondmtheethiropdrso[d2u6c].tiTohnempeottheondtisa[l2v6a].luTeheofpiostoelnateiadl vCaNluFewofaisoalsastesdseCdNiFnwoardsearssteossmedeaisnuorredietsrtsotambeilaitsyur[e27it]s.sTtahbeilziteyta[2p7o].teTnhteiazleatanpaloytseenstioafl bamboo CNF and commercial CNF are presented in Figure 1e,f, respectively. The potential analyses of bamboo CNF and commercial CNF are presented in Figure 1e,f, respectively. of each type of CNF had values ranging between 0 and 50 V. Previous reports on zeta The potential of each type of CNF had values ranging between 0 and 50 V. Previous re‐ potential analysis show that a potential above 20 V is considered stable in the colloidal ports on zeta potential analysis show that a potential above 20 V is considered stable in fluid [28,29]. Since both CNF were higher than 20 V, the high voltage indicated stable the colloidal fluid [28,29]. Since both CNF were higher than 20 V, the high voltage indi‐ particle materials. These results confirmed that the isolated CNF could not be modified cated stable particle materials. These results confirmed that the isolated CNF could not be back to its raw material or have its properties changed, even at high voltage. This means modified back to its raw material or have its properties changed, even at high voltage. that the isolation process produced a stable cellulose nanofibre [29]. This means that the isolation process produced a stable cellulose nanofibre [29]. The results of the FT-IR, XRD, and TGA-DTG analyses of the bamboo and the com- The results of the FT‐IR, XRD, and TGA‐DTG analyses of the bamboo and the com‐ mercial CNF are presented in Figure 2a–d. mercial CNF are presented in Figure 2a–d. a) 1.2 1.0 0.8 0.6 0.4 0.2 c) 100 90 80 70 60 50 3400 2950 Commercial CNF Bamboo CNF 1641 1050 560 1375 b) 2500 2000 1500 1000 500 Commercial CNF Bamboo CNF 4000 3500 3000 2500 2000 1500 1000 500 Wave number (cm‐1) 0 10 20 30 40 50 60 70 2 Theta Bamboo CNF Commercial CNF d) 0.000 ‐0.004 ‐0.008 ‐0.012 ‐0.016 30 20 10 89 150 200 Temperature (C) 250 300 Weight loss (%) Weight loss (%) Derivative weight loss (1/ C) Intensity (counts) Derivative weight loss (mg/ C) Absorbance (a.u.) 0 0 100 200 300 400 500 600 700 800 0 100 200 300 400 500 600 700 800 900 93 92 91 Bamboo CNF Commercial CNF 40 90 ‐0.014 ‐0.016 340 350 Temperature (C) Figure 2. Results obtained from bamboo and commercial CNFs by (a) FT‐IR; (b) XRD; (c) TGA; and (d) DTG. Temperature (C) Figure 2. Results obtained from bamboo and commercial CNFs by (a) FT-IR; (b) XRD; (c) TGA; and (d) DTG. Both FT-IR bands (Figure 2a) showed a wavenumber band of 3600–3200 cm−1, sug- gesting the stretching of hydroxide, corresponding to hydrogen bonds in the structure (-H of the –OH group). The wavenumber band at 2969 cm−1 and 2902 cm−1 corresponds to 360 370 380 390 400 Temperature (C)PDF Image | Supercritical Carbon Dioxide Isolation of Cellulose Nanofibre
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