Synthesis evidence

Thin film thermoelectric metal-organic framework with high seebeck coefficient and low thermal conductivity

Erickson K.J., Leonard F., Stavila V. et al. · Advanced Materials · 2015 · 3453-3459

3 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

main p.6, article p.3458 · Growth and Characterization of MOF Thin Films

Metal precursorsNot specified in this paper; Cu3(BTC)2 liquid-phase layer-by-layer film growth cited to a previously described procedure.
Linker precursorsNot specified in this paper; BTC linker implied by Cu3(BTC)2.
SolventsLiquid phase; solvent not specified for framework growth in this paper.
AtmosphereVacuum only specified for activation, about 10^-6 Torr.
Temperatureroom temperature deposition described generally; activation at 180 deg C
Timeactivation 1 h; growth time not specified
Substrate orientationFused quartz substrate with prepatterned Au pads; no crystal orientation specified for substrate.
Work-upNot specified for growth; residual solvent and precursors removed by heating before infiltration.
ActivationHeated at 180 deg C in vacuum (about 10^-6 Torr) for 1 h before TCNQ infiltration.
Scalability contextAutomated layer-by-layer approach; grain size varies from tens of nanometres to about 1 um depending on film thickness and growth conditions.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu source not specified in this paperNot specifiedmain p.6, article p.3458 · Growth and Characterization of MOF Thin Films
LinkerBTC linker implied; exact reagent not specified in this paperNot specifiedmain p.6, article p.3458 · Growth and Characterization of MOF Thin Films
Otherfused quartz substrate with prepatterned Au pads19 x 19 mm2, 0.55 mm thick; Au pads 200 x 500 ummain p.6, article p.3458 · Growth and Characterization of MOF Thin Films
Vague recipeSource: Main

Route 2: Other

main p.6, article p.3458 · Thermal Conductivity Measurements · Figure 4

Metal precursorsPreformed Cu3(BTC)2 film; detailed Cu source not specified.
Linker precursorsBTC framework linker and TCNQ guest molecule; detailed framework-growth reagent names not specified.
SolventsTCNQ infiltration solvent inferred from similar method as methanol; growth solvent not specified.
Substrate orientationp-Si wafer coated with 100 nm thermal oxide; patterned Au pads for conductivity measurements.
Oxidant / reductantTCNQ redox-active guest molecule
Work-up200 nm thick, 0.75 mm diameter Al dots deposited on top for TDTR measurements.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otherp-Si wafer coated with 100 nm thermal oxideNot specifiedmain p.6, article p.3458 · Thermal Conductivity Measurements · Figure 4
OtherAl TDTR transducer dots200 nm thick, 0.75 mm diametermain p.6, article p.3458 · Thermal Conductivity Measurements · Figure 4
Partial recipeSource: Main

Route 3: Other

main p.6, article p.3458 · Growth and Characterization of MOF Thin Films · Figure 1

Metal precursorsPreformed Cu3(BTC)2 thin film.
Linker precursorsTCNQ guest molecule; BTC already present in framework.
SolventsMethanol
AtmosphereN2 stream used for drying; infiltration atmosphere not specified.
Temperatureroom temperature
Timeabout 24 h infiltration
Substrate orientationDevice held vertically in a glass bottle by side ridges; roughly lower half immersed in TCNQ/methanol.
Oxidant / reductantTCNQ redox-active guest molecule
Work-upRemoved after about 24 h, rinsed with methanol, dried under a stream of N2.
ActivationImmediately before infiltration, residual solvent and precursors were removed by heating at 180 deg C in vacuum (about 10^-6 Torr) for 1 h.
Scalability contextPartial immersion creates infiltrated, transition and uninfiltrated regions in the same device.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otherpreformed activated Cu3(BTC)2 thin film200 nm nominal film on quartzmain p.6, article p.3458 · Growth and Characterization of MOF Thin Films · Figure 1
OxidantTCNQ (tetracyanoquinodimethane)saturated solution in methanolmain p.6, article p.3458 · Growth and Characterization of MOF Thin Films · Figure 1
SolventmethanolNot specifiedmain p.6, article p.3458 · Growth and Characterization of MOF Thin Films · Figure 1