cMOF Evidence Base

Synthesis evidence

Layer-by-Layer Assembled Conductive Metal–Organic Framework Nanofilms for Room-Temperature Chemiresistive Sensing

Yao M.-S., Lv X.-J., Fu Z.-H. et al. · Angewandte Chemie - International Edition · 2017 · 16510-16514

3 structured synthesis routes

Completeness describes how fully the route could be reconstructed from the main article and supporting information.

Partial recipeSource: Both

Route 1: Other

SI p.1-p.2 · Fabrication of Cu3(HHTP)2-xC thin film

Metal precursorsCopper acetate / copper(II) acetate, reported as Cu(OAc)2.H2O in SI and 0.1 mM ethanolic copper acetate solution for spraying.
Linker precursorsHHTP, 2,3,6,7,10,11-hexahydroxytriphenylene, 0.01 mM ethanolic solution.
SolventsEthanol for metal solution, linker solution, rinse and MUD SAM; acetone, ethanol and DI water used in substrate cleaning.
Additives11-Mercapto-1-undecanol (MUD) used to form OH-functionalized SAMs on Au; piranha solution used to hydroxylate oxide substrates.
AtmosphereN2 stream/flux for drying functionalized substrates and final thin films; spray atmosphere not specified.
Temperature100 C for piranha treatment; spray deposition temperature not specified.
TimePiranha treatment 1 h; MUD SAM immersion 24 h; 20 s copper acetate spray and 40 s HHTP spray per cycle; number of cycles x defines xC sample.
Substrate orientationFunctionalized sapphire, glass, Si/SiO2, quartz, Si/Au or Au-interdigitated substrates; no crystallographic orientation specified.
Oxidant / reductantPiranha solution H2SO4 (95%-98%) / H2O2 (30%) = 7:3 for substrate hydroxylation.
Work-upBetween spray steps the substrate was rinsed/sprayed with pure ethanol to remove residual reactants; films dried by N2.
ActivationNo post-synthetic activation beyond N2 drying is reported.
Scalability contextLayer-by-layer spray process gives about 2 nm thickness increment per cycle and allows xC thickness control, but spray volume/rate and ambient deposition conditions are not reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate / Cu(OAc)2.H2O0.1 mM in ethanolSI p.1-p.2 · Fabrication of Cu3(HHTP)2-xC thin film
LinkerHHTP (2,3,6,7,10,11-hexahydroxytriphenylene)0.01 mM in ethanolSI p.1-p.2 · Fabrication of Cu3(HHTP)2-xC thin film
SolventethanolNot specifiedSI p.1-p.2 · Fabrication of Cu3(HHTP)2-xC thin film
Additive11-Mercapto-1-undecanol (MUD)1 mM ethanolic solution for Au SAMSI p.1-p.2 · Fabrication of Cu3(HHTP)2-xC thin film
OxidantPiranha solution H2SO4 (95%-98%) / H2O2 (30%) = 7:3Not specifiedSI p.1-p.2 · Fabrication of Cu3(HHTP)2-xC thin film
Vague recipeSource: SI

Route 2: Drop Cast

SI p.3 · Gas sensor characterizations · Figure S7

Substrate orientationSensor substrate not specified.
Complete recipeSource: SI

Route 3: Solvothermal

SI p.2 · Preparation of Cu3(HHTP)2 powders

Metal precursorsCopper acetate, 6.4 mg in 2 mL methanol.
Linker precursorsHHTP, 5.2 mg in 2.5 mL methanol.
SolventsMethanol.
AtmosphereSealed glass bottle; drying under vacuum.
Temperature65 C reaction; 100 C vacuum drying.
TimeStirred 5 min; heated 24 h; vacuum dried 12 h.
Work-upProducts collected from bottom of reactor; washed four times with fresh methanol by dispersion and centrifugation.
ActivationDried in vacuum at 100 C for 12 h.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate6.4 mg in 2 mL methanolSI p.2 · Preparation of Cu3(HHTP)2 powders
LinkerHHTP5.2 mg in 2.5 mL methanolSI p.2 · Preparation of Cu3(HHTP)2 powders
Solventmethanol4.5 mL total reported solution volumeSI p.2 · Preparation of Cu3(HHTP)2 powders