cMOF Evidence Base

Synthesis evidence

Layer-by-layer assembled dual-ligand conductive MOF nano-films with modulated chemiresistive sensitivity and selectivity

Wu A.-Q., Wang W.-Q., Zhan H.-B. et al. · Nano Research · 2021 · 438-443

2 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

p002 / article p.439 · Results and discussion · Fig. 2(b)

Metal precursorsCopper acetate implied by the shared Cu-HHTP spray LbL chemistry
Linker precursorsHHTP; no HITP dopant for pristine comparator
Solventsethanol likely, by analogy to doped-film recipe
Additivesnot separately reported
Atmospherenot separately reported
Time10 cycles implied by '-10C' naming
Substrate orientationOH-functionalised substrate
Work-upnot separately reported for pristine comparator
Activationnot separately reported for pristine comparator
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate, implied from adjacent doped-film recipeNot specifiedp002 / article p.439 · Results and discussion · Fig. 2(b)
LinkerHHTPNot specifiedp002 / article p.439 · Results and discussion · Fig. 2(b)
Complete recipeSource: Both

Route 2: Other

p001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film

Metal precursorscopper acetate (Cu(OAc)2.H2O), 0.1 mM ethanolic solution
Linker precursorsHHTP (0.01 mM) and HITP (0.1 mM) mixed ethanolic solution; molar ratio varied to obtain x = 0.1, 0.5, 1.0, 5.0 and 10.0 mol% expected HITP dopants
Solventsethanol for precursor solutions and rinsing; DMF and ethanol for activation; acetone, ethanol and DI water for substrate cleaning
Additivesammonium hydroxide (28%) to regulate mixed-ligand solution to pH 8.5; MUD for Au substrate OH-functionalised SAM; Piranha solution for oxide substrates
AtmosphereSubstrates and films dried under N2/N2 flux; deposition atmosphere otherwise not specified
Temperature100 degC for Piranha cleaning; room temperature for SAM formation and DMF/ethanol activation; deposition temperature not specified
TimeMUD SAM 24 h; Piranha 1 h; post-Piranha ultrasonic ethanol 0.5 h; LbL cycle uses 20 s copper acetate spray, 40 s mixed-linker spray and 20 s steady growth after every spray for 10 cycles; DMF activation 2 h and ethanol activation 12 h
Substrate orientationFunctionalised sapphire (8 x 10 x 1 mm3), Si/SiO2, quartz, glass, silicon wafer, or Au-coated/interdigital-electrode substrates; OH-functionalised surfaces used to facilitate growth
Oxidant / reductantPiranha solution H2SO4/H2O2 = 7:3 for substrate cleaning; no framework oxidant/reductant specified
Work-upBetween each spray step, rinse substrate with pure ethanol to remove residual reactants; after 10 cycles dry films by N2.
ActivationSuccessive immersions in N,N-dimethylformamide (DMF, 2 h) and ethanol (12 h) at room temperature, followed by drying by N2.
Scalability contextSpray LbL gives nanometre-scale control but no scale-up experiment is reported.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper acetate (Cu(OAc)2.H2O)0.1 mM in ethanolp001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
LinkerHHTP0.01 mM in mixed ethanolic solutionp001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
LinkerHITP (2,3,6,7,10,11-hexamminetriphenylene as printed in SI)0.1 mM in mixed ethanolic solutionp001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
Baseammonium hydroxide28%; used to regulate pH to 8.5p001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
Solventethanolprecursor solvent and pure ethanol rinsep001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
SolventN,N-dimethylformamide (DMF)activation immersion, 2 hp001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
Additive11-mercapto-1-undecanol (MUD)Au substrates immersed 24 h · 1 mM ethanolic solutionp001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film
AcidPiranha solution H2SO4 (95%-98%) / H2O2 (30%) = 7:3oxide substrates immersed at 100 degC for 1 hp001 / SI p.1 · Fabrication of HITP doped Cu3(HHTP)2-10C thin film