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Materials 2021, 14, 1786 15 of 20 Materials 2021, 14, 1786 15 of 19 The PL properties of Sm- and Tb-based CPs were investigated at room temperature intheTshoelidPLstpartoepaesrtpieoswodfeSrms-oarnednTcabp-bsausleadteCdPisnwPeMreMinAve(sFtigautreed9a)t.rIonogmentemrapl,erthateuresults obintatihneesdolbidysthtaetetwasopmowetdheordssorwenrceaspismuilalater,dthinuPsMonMlyAth(Feigreusruel9ts).oInbtgaeinerdalw,tihthertheseuPltMsMA enobcatapinsuedlabtiyotnhemtwetohmodetwhoidllsbweepreressimeniltaerd,/thduiscounslysethde.rTehsueltflsuoobtraeisncednwceitihntheenPsiMtyMaAndPL liefentciampesuplatriaomn metetrhsoadrewsiullmbempareriszeendteidn/dTiascbuless6e,da. nTdhethfleuoarneaslcyesnicseoinf tehnesietyraensudlPtsLilnifdei-cates 3.4. Photoluminescence Studies 3.4. Photoluminescence Studies time parameters are summarized in Table 6, and the analysis of these results indicates that that there are significant differences between all the CPs, demonstrating the effect of the there are significant differences between all the CPs, demonstrating the effect of the crys- crystalline structure features in the PL properties. talline structure features in the PL properties. Figure 9. Schematic illustration of the powder (left side) and PMMA encapsulation (right side) Figure 9. Schematic illustration of the powder (left side) and PMMA encapsulation (right side) methods used for the study of the PL properties. methods used for the study of the PL properties. The PL properties of SmCP1 and TbCP1 prepared by HT and MWAS were similar Table 6. PL peak wavelengths and PL decay parameters of all the CPs prepared by HT and MWAS. CP SmCP1 TbCP1 TbCP2 between the two synthetic methodologies. Nevertheless, for TbCP1 a decrease in the life- time value of ≈20% is observed from HT to MWAS materials. The comparison of the life- Synthesis Method λem/nm τx/μs (%)(a) τtotal(b)/μs X2(c) time values of SmCP1 and TbCP1 (Table 3)—4.43 μs vs. 185.57 μs (HT) and 4.39 μs vs. HT MWAS HT MWAS HT 590 (max), 148.15 μs (MWAS), respectively—indicates that the energy transfer from ligand, CP1, to 483, 493, 518, 560, 565, 605, 642, 649, 698 4.43 (100) 4.43 1.015 Tb3+ metal center is much more efficient than to Sm3+ metal center. It is clear the importance 596 (max), of the selection of the metal center in the preparation of luminescent CP. Regarding TbCP2 482, 492, 519, 559, 565, 605, 642, 648, 697 4.39 (100) 4.39 1.000 and TbCP3, only one set of data was collected since these materials were obtained using only HT synthesis. The “exchange” of the coordinated H2O molecules in TbCP2 for a phen 492, 545 (max), 43.82 (10.09) 185.57 1.001 molecule in55T1,b5C83P,358l9e,d62t2o,6a47s,i6g6n8,if6i8c0ant change in the PL properties, particularly in the lifetime value. The lifetime value of TbCP3 is 6.8 times higher than that of TbCP2. 278.43 (27.95) 136.121 (50.14) 283.94 (39.76) The Sm3+ CP showed relatively narrow emission peaks corresponding to the expected 492, 545 (max), 121.331 (50.30) 148.15 1.004 3+ transitions 5a5s0s,o5c8i4a,t5e8d9,w62it2h, 6S4m8, 66(8F, i6g8u0re 10A). PL e4x3c.6i6ta2t(i2o1n.24sp) ectra and the graphical rep- resentations of the PL intensity in function of lifetime are included in the Supplementary Material (Figure S7). All the Tb3+ CP showed ident1ic37a.l9n11ar(2r9o.w53)emission peaks (Figure 10B– 5.13 (0.50) 489, 543 (max), 64.737 (57.72) 80.85 1.049 D), with very small deviations in the emission wavelengths (Table 6), corresponding to 548, 588, 620, 647 21.626 (12.76) the 5D4 →7FJ (J = 6–2) transitions of Tb3+ ion, with the maximum peaks at 545/543 and 546 696.22 (76.77) 5 7 HT nm respectively, which could be ascribed to the contribution from the D4 → F5 transition. 490, 546 (max), 0.771 (0.25) The spectra and data presented are very similar to those reported by Sa5r4m6.9a9and co-w0o.r9k75- TbCP3 a PL decay measured at the maximum emission peaks of each material. b Total lifetime (τtotal) of each material is given by intensity weighted lifetime. c noteworthy difference between the CP luminescence spectra is the presence of two addi- 2 tional transitions for TbCP1 relative to TbCP3, corresponding to the 5D4 →7FJ (J = 1–0) 586, 622, 650 25.186 (15.96) ers [45], including those of lifetime values (approximately 100 μs) for the 1D CP. The more 120.87 (7.02) X indicates the goodness of the fitting results. transitions of the Tb3+ ion; on the other hand, the resolution of the TbCP2 spectrum does not allow for the observation of such transitions with certainty (the very noisy part of the The PL properties of SmCP1 and TbCP1 prepared by HT and MWAS were similar spectrum is caused by the instrument of the exciting wavelength). The PL excitation spec- between the two synthetic methodologies. Nevertheless, for TbCP1 a decrease in the tra of TbCP1 and TbCP3 (Supplementary Material: Figure S8) revealed a broad band with lifetime value of ≈20% is observed from HT to MWAS materials. The comparison of the a maximum at approximately 390 nm, which can be associated with the intra-ligand tran- lifetime values of SmCP1 and TbCP1 (Table 3)—4.43 μs vs. 185.57 μs (HT) and 4.39 μs vs. sitions of the H2aip ligand, as reported in related compounds [24,45]. The presence of the 148.15 μs (MWAS), respectively—indicates that the energy transfer from ligand, CP1, to Tb3+ metal center is much more efficient than to Sm3+ metal center. It is clear the importancePDF Image | Green Chemistry with Supercritical CO2 and Enzymes
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