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 | |
Nonapplicable entries are indicated as NA.