Synthesis evidence

Tunable electrical conductivity in metal-organic framework thin-film devices

Talin A.A., Centrone A., Ford A.C. et al. · Science · 2014 · 66-69

6 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Other

3 · main text · Fig. 2A

Metal precursorspreformed Cu3(BTC)2 thin film
Linker precursorsBTC already present in host film
AdditivesF4-TCNQ
Substrate orientationPt/SiO2 device wafer
Oxidant / reductantF4-TCNQ guest
Activationhost activation presumed from TCNQ route but not independently specified
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(BTC)2 thin-film deviceNot specified3 · main text · Fig. 2A
OxidantF4-TCNQNot specified3 · main text · Fig. 2A
Vague recipeSource: Both

Route 2: Other

3 · Elemental Analysis · Table S1

Metal precursorspreformed Cu3(BTC)2
Linker precursorsBTC already present in host framework
SolventsCH2Cl2 residual solvent indicated for powder
AdditivesH4-TCNQ
Oxidant / reductantH4-TCNQ guest
Activationhost activation presumed but not independently specified
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(BTC)2Not specified3 · Elemental Analysis · Table S1
OtherH4-TCNQNot specified3 · Elemental Analysis · Table S1
SolventCH2Cl2residual 1/3 CH2Cl2 in formula model3 · Elemental Analysis · Table S1
Partial recipeSource: Main

Route 3: Other

1 · main text

Substrate orientationPt pads on Si wafer with 100 nm SiO2; electrode gaps 100, 150, 200 um
Scalability contextThin films grown directly on prepatterned device wafers.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenot specified in this paperNot specified1 · main text
Linkerbenzene-1,3,5-tricarboxylic acid implied by BTC frameworkNot specified1 · main text
Partial recipeSource: SI

Route 4: Other

2 · Figure S1 caption · Fig. S1

Metal precursorsCu3(BTC)2.xH2O powder
Linker precursorsBTC in preformed framework
Atmospherevacuum
Temperature180
Time0.5
Activationheating to 180 C for 30 min under vacuum
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherCu3(BTC)2.xH2O powderNot specified2 · Figure S1 caption · Fig. S1
Partial recipeSource: Main

Route 5: Other

1 · main text · Fig. 2A

Metal precursorspreformed Cu3(BTC)2 thin film
Linker precursorsBTC already present in host film
SolventsCH2Cl2
AdditivesTCNQ guest molecule
Atmospherevacuum during activation; exposure solution atmosphere not specified
Temperature190
Time0.5 h vacuum activation; 72 h TCNQ exposure for reported Fig. 2A devices
Substrate orientationPt/SiO2 device wafer
Oxidant / reductantredox-active TCNQ guest
Work-upimmediate transfer to saturated TCNQ/CH2Cl2 solution; subsequent drying in air noted for powder BET material
Activationheated in vacuum at 190 C for 30 min to remove coordinated water
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(BTC)2 thin-film deviceNot specified1 · main text · Fig. 2A
Oxidant7,7,8,8-tetracyanoquinododimethane (TCNQ)saturated solution · saturated in CH2Cl21 · main text · Fig. 2A
SolventCH2Cl2Not specified1 · main text · Fig. 2A
Vague recipeSource: Both

Route 6: Other

2 · main text · Fig. 1C; Table S1

Metal precursorspreformed activated Cu3(BTC)2 powder
Linker precursorsBTC already present in host framework
SolventsCH2Cl2 inferred from film infiltration and Table S1 H4 solvent note; powder solvent not explicitly stated
AdditivesTCNQ
Oxidant / reductantredox-active TCNQ guest
Work-updrying in air before BET measurement
Activationactivated host required to expose open metal sites
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated Cu3(BTC)2 powderNot specified2 · main text · Fig. 1C; Table S1
OxidantTCNQNot specified2 · main text · Fig. 1C; Table S1