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. 2019 Sep 26;4(15):16257–16269. doi: 10.1021/acsomega.9b00491

Table 3. Description of Synthesis Steps for Synthetic Gel Batches Corresponding to Steps a–i in Figure 1a.

 
CJ2
CJ3
ISG
label synthesis steps CJ2.3.B CJ2.3.E CJ2.7.B CJ2.9.A CJ2.9.B CJ3.3.B CJ3.7.A CJ3.9.A ISG.3.B ISG.7.A ISG.9.B
a ethanol (mL) 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50
  H2O (mL) 0.424 0.424 0.424 0.424 0.424 0.424 0.424 0.424 0.424 0.424 0.424
  TEOS (mL) 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00 5.00
  catalyst 0.22 mL of 0.1 M HNO3 0.25 mL of 0.1 M HNO3 NA NA NA 0.44 mL of 0.1 M HNO3 18 μL of 0.1 M NH4OH/NH4F NA 0.22 mL of 0.1 M HNO3 18 μL of 0.1 M NH4OH/NH4F 40 μL of conc. NH4OH
  pH 4 3.5 NA 5 NA 3 7 NA 3 6.5–7 8–8.5
  mixing time (h) 5.5 6.5 5.5 7 7 22.5 ∼6 7 24 8 5
                         
b ethanol (mL) 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50 5.50
  Al(OBus)3 (mL) 0.801 0.801 0.801 0.800 0.800 0.860 0.860 0.860 0.842 0.814 1.544
  Zr(IV) prop (mL) NA NA NA NA NA NA NA NA 0.240 0.288 0.580
                         
c mixing time (h) 18 6.5 18 18 19 21 11.25 18 23 18.75 17
  pH after mixing NA NA NA NA NA 1 NA NA 1–1.5 2 1.5
                         
d CaMeEt (mL) NA NA NA NA NA 2.90 2.290 2.290 0.906 0.906 2.438
  NaOEt (mL) 1.586 1.586 1.586 1.586 1.586 0.528 0.528 0.528 1.358 1.598 0.878
                         
e mixing time (h) 6 12.15 6 5.5 5.75 5.5 21.75 22.25 27 7.5 31
  pH after mixing NA NA NA NA NA 8 NA 6.25 8 11 11
                         
f gelling agent 0.19 mL of 0.10 M HNO3, 0.8 mL of conc HNO3, 1.271 mL of H2O 1.020 mL of H2O 17 μL of NH4OH/NH4F 0.3 mL of NH4OH/NH4F, 1.271 mL of H2O 1.270 mL of H2O 1.251 mL of H2O 1.271 mL of H2O 1.10 mL of NH4OH/NH4F, 1.271 mL of H2O 1.271 mL of 0.1 M HNO3 1.254 mL of 0.1 M HNO3 1.572 mL of H2O
                         
g pH after gelling agent addition 3.25 7 11 10 8.5 8 7 8.75 8 10.5 9
                         
h gelation time (days) 19 5 7.25 0 0 2 7 9 1 10.5 1
                         
i aging time (days)                      
  i.1 7 7 1 3 14 7 17 3 7 15 30
  i.2 31 30 3 7 30 15 17 7 15 49 45
  i.3 45 61 15 15 45 45 17 15 47 60 75
  i.4 60 75 60 30 76 60 30 30 60 75 90
  1.5 NA NA NA NA NA NA 45 90 NA NA NA
a

Nonapplicable entries are indicated as NA.