Complete recipeSource: Both
Route 1: Other
p004 · 1.3 Fabrication of Cu-HHTP-xC films
Metal precursorsCopper acetate (Cu(OAc)2.H2O), 0.1 mM ethanolic solution
Linker precursorsHHTP (2,3,6,7,10,11-hexahydrotriphenylene / hexahydroxytriphenylene), 0.01 mM ethanolic solution
Solventsethanol for Cu acetate and HHTP spray solutions and rinse; acetone, ethanol and deionized water for substrate cleaning; piranha solution H2SO4/H2O2 for hydroxyl functionalisation
Additivesnone reported for MOF growth
Atmosphereambient spray process controlled at 25 deg C and 40 %RH; N2 stream drying between spray steps
Temperature25
TimePer growth cycle: copper acetate spray 20 s, ethanol rinse 40 s and N2 dry 20 s; HHTP spray 40 s, ethanol rinse 40 s and N2 dry 20 s; repeated x = 1-60 cycles.
Substrate orientationSapphire substrates (2 x 1 x 1 mm3), silicon wafers and SiO2 (300 nm)-coated silicon wafers; hydroxyl-functionalised before growth; Cr/Au electrodes with 10 um channel width on sapphire for device measurements.
Oxidant / reductantPiranha solution H2SO4 (95%-98%) / H2O2 (30%) = 7:3 used for substrate functionalisation; no oxidant/reductant reported in MOF spray growth.
Work-upSubstrates alternately ultrasonicated in acetone, ethanol and DI water; immersed in piranha solution at 100 deg C for 1 h; rinsed and ultrasonically cleaned 30 min in ethanol; dried under N2. During growth, ethanol spray rinses remove residual reactants after each precursor spray, followed by N2 drying.
ActivationNo general activation reported for as-grown xC series; XRD specimens received separate HHTP immersion described in route r_xrd_hhtp_crystallinity_treatment.
Scalability contextSpray LBL-LPE uses 15 sccm/min precursor flow and is repeated to tune film thickness by growth cycle number.
Show 7 structured reagent records
| Role | Reagent | Amount / concentration | Source |
|---|---|---|---|
| Metal Source | Copper acetate (Cu(OAc)2.H2O), purchased from Sigma Aldrich | sprayed for 20 s per growth cycle at 15 sccm/min · 0.1 mM ethanolic solution | p004 · 1.3 Fabrication of Cu-HHTP-xC films |
| Linker | HHTP (2,3,6,7,10,11-hexahydrotriphenylene), purchased from TCI (Shanghai) | sprayed for 40 s per growth cycle at 15 sccm/min · 0.01 mM ethanolic solution | p004 · 1.3 Fabrication of Cu-HHTP-xC films |
| Solvent | ethanol | 40 s rinse between each spray step; also solvent for precursor solutions · pure ethanol for rinse | p004 · 1.3 Fabrication of Cu-HHTP-xC films |
| Solvent | acetone, ethanol and deionized water | alternate ultrasonication substrate cleaning | p004 · 1.3 Fabrication of Cu-HHTP-xC films |
| Acid | H2SO4 | piranha solution H2SO4/H2O2 = 7:3, 100 deg C for 1 h · 95%-98% | p004 · 1.3 Fabrication of Cu-HHTP-xC films |
| Oxidant | H2O2 | piranha solution H2SO4/H2O2 = 7:3, 100 deg C for 1 h · 30% | p004 · 1.3 Fabrication of Cu-HHTP-xC films |
| Other | N2 gas | 20 s drying after ethanol rinse | p004 · 1.3 Fabrication of Cu-HHTP-xC films |