cMOF Evidence Base

Synthesis evidence

Anisotropic Redox Conductivity within a Metal-Organic Framework Material

Goswami S., Hod I., Duan J.D. et al. · Journal of the American Chemical Society · 2019 · 17696-17702

2 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Electrochemical

4 · Electrophoretic deposition of NU-1000

Metal precursorsBulk NU-1000 powder contains Zr6 nodes; bulk synthesis not reproduced
Linker precursorsBulk NU-1000 powder contains H4TBAPy-derived linkers; bulk synthesis not reproduced
Solventstoluene
AdditivesZnO-coated FTO substrates
Atmospherenot specified
Temperatureroom temperature implied for electrophoretic deposition
Timeabout 3 h deposition; about 30 s sonication
Substrate orientationTwo ZnO-coated FTO substrates dipped in MOF suspension with about 1 cm separation distance.
Oxidant / reductantconstant DC voltage about 136 V
Work-upnot specified after deposition
Activationnot specified for EPD film after deposition
Scalability contextDeposition performed between two ZnO-coated FTO substrates separated by about 1 cm.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherbulk NU-1000 powder10 mg4 · Electrophoretic deposition of NU-1000
Solventtoluene20 mL4 · Electrophoretic deposition of NU-1000
OtherZnO coated FTO substratestwo substrates4 · Electrophoretic deposition of NU-1000
Complete recipeSource: SI

Route 2: Solvothermal

3-4 · Synthesis of NU-1000 solvothermal films

Metal precursorszirconyl chloride octahydrate (105 mg)
Linker precursorsH4TBAPy, 0.5 mM DMF pretreatment solution and 40 mg added to growth solution
SolventsDMF; substrate washing with soapy water, water, ethanol and acetone; acetone workup
Additivesbenzoic acid (2.7 g); ZnO barrier layer from ALD diethylzinc/steam cycles; dilute hydrochloric acid/DMF activation solution
Atmospherenot specified
TemperatureFTO drying 100 C; ZnO ALD about 150 C; Zr/benzoic acid preheat 80 C for 2 h; MOF growth 90 C for 18 h; activation 100 C for 4 days
TimeFTO sonication washes 0.25 h each; drying 0.5 h; linker pretreatment 12 h; preheat 2 h; MOF growth 18 h; activation 96 h
Substrate orientationPretreated FTO substrates placed with conductive surface facing downwards; product on conductive side.
Work-upCooled to room temperature; FTO substrate washed with DMF to remove precipitate; after activation thoroughly washed with acetone and dried under vacuum.
ActivationCoordinated benzoates removed by soaking MOF thin film in dilute HCl/DMF solution for 4 days at 100 C, followed by acetone washing and vacuum drying.
Scalability contextPrepared on 3 cm x 1.25 cm FTO glass substrates.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcezirconyl chloride octahydrate105 mg3-4 · Synthesis of NU-1000 solvothermal films
LinkerH4TBAPy40 mg in growth solution; pretreatment used 0.5 mM solution · 0.5 mM in DMF for substrate pretreatment3-4 · Synthesis of NU-1000 solvothermal films
SolventN,N-dimethylformamide (DMF)8 mL for growth solution; 13 mL and 50 mL used in activation dilution3-4 · Synthesis of NU-1000 solvothermal films
Additivebenzoic acid2.7 g3-4 · Synthesis of NU-1000 solvothermal films
Acidhydrochloric acid0.5 mL of 8 M HCl combined with 13 mL DMF; 0.05 mL of this solution mixed with 50 mL DMF · 8 M stock3-4 · Synthesis of NU-1000 solvothermal films
Otherdiethylzinc (DEZ) and steamfive AB ALD cycles3-4 · Synthesis of NU-1000 solvothermal films