Synthesis evidence

High performance metal–organic-framework coatings obtained via thermal gradient synthesis

Jeremias F., Henninger S.K., Janiak C. · Chemical Communications · 2012 · 9708-9710

1 structured synthesis route

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

Complete recipeSource: Both

Route 1: Other

1-2 · Synthesis / Experimental procedure · Figure S1

Metal precursorsCu(NO3)2 . 3 H2O (>=98%, Carl Roth), 7.00 g, 28.09 mmol; possible minor contribution from Cu sheet/oxide is discussed but substrate plays a minor role
Linker precursorstrimesic acid / H3btc (98%, ABCR), 3.36 g, 15.99 mmol
Solventsredistilled DMF, 200 ml; activation/washing with DMF and redistilled ethanol
Additivesnone reported; optional acetone degreasing before sanding had no effect; SiC CAMI grit 600 used for wet sanding
AtmosphereCopper-sheet tempering in air; reaction atmosphere not explicitly specified; sample stored under inert conditions after drying
Temperature150 deg C at Cu sheet/heater interface during growth; stirred ice-water bath around solution; pre-tempering 150 deg C for 12 h in SI, but main text says 120 deg C for 12 h
Time2 h coating growth; 12 h DMF activation soak; two ethanol soaks; dried overnight at 120 deg C
Substrate orientationPrepared Cu sheets attached to both sides of heating block and immersed in stirred Cu(NO3)2-H3btc-DMF solution; interface thermocouple at heater/copper sheet interface
Oxidant / reductantDMF is discussed as a reducing agent at elevated temperature if H2O is present; multicoloured oxide layer disappeared at experiment start
Work-upCoated sheet rinsed with DMF, immersed in DMF for 12 h, then the procedure was repeated twice with redistilled ethanol
ActivationDry in air at 120 deg C overnight and store under inert conditions after solvent exchange
Scalability context5 cm x 5 cm Cu support, 25 cm2, could be enlarged; reproducibility within 3% over six preparations; successful layer formation also observed on aluminium and stainless steel sheets.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2 . 3 H2O (>= 98%, Carl Roth)7.00 g (28.09 mmol) · in 200 ml DMF1-2 · Synthesis / Experimental procedure · Figure S1
Linkertrimesic acid / H3btc (98%, ABCR)3.36 g (15.99 mmol) · in 200 ml DMF1-2 · Synthesis / Experimental procedure · Figure S1
Solventdimethyl formamide / DMF (>=99.5%, Carl Roth), redistilled200 ml1-2 · Synthesis / Experimental procedure · Figure S1
OtherETP copper sheets50 mm x 50 mm x 0.60 mm sheets1-2 · Synthesis / Experimental procedure · Figure S1
Solventredistilled ethanoltwo immersion repetitions1-2 · Synthesis / Experimental procedure · Figure S1
Otheracetoneoptional degreasing before sanding1-2 · Synthesis / Experimental procedure · Figure S1