Synthesis evidence

A one-dimensional conductive metal-organic framework with extended π-d conjugated nanoribbon layers

Shang S., Du C., Liu Y. et al. · Nature Communications · 2022 · 7599

4 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

7 · Methods - Synthesis of DDA-Cu MOF crystals

Metal precursors22.2 mg Cu(CH3COO)2·H2O in 400 mL ethanol + 100 mL water (solution B)
Linker precursors30 mg DDA in 400 mL ethanol + 100 mL water (solution A)
Solventsethanol and water
Additivesacetate from copper acetate; no separate additive reported
Atmospherenormal pressure; ambient oxygen involved in amino oxidation mechanism
Temperature90
Time24
Substrate orientationnone
Oxidant / reductantO2 in air oxidises amino groups; deprotonation/oxidation mechanism in SI
Work-upsolution A sonicated 30 min; solution B added at about 2 drops/s under stirring; centrifuged at 9000 rpm; washed/centrifuged with ethanol and water until supernatant clear
Activationvacuum oven drying at 90 C for 12 h
Scalability contextisolated yields 85-92%
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerDDA30 mg · 400 mL ethanol + 100 mL water7 · Methods - Synthesis of DDA-Cu MOF crystals
Metal SourceCu(CH3COO)2·H2O22.2 mg · 400 mL ethanol + 100 mL water7 · Methods - Synthesis of DDA-Cu MOF crystals
Solventethanol800 mL total7 · Methods - Synthesis of DDA-Cu MOF crystals
Solventwater200 mL total7 · Methods - Synthesis of DDA-Cu MOF crystals
OxidantO2 / airnot quantified · ambient7 · Methods - Synthesis of DDA-Cu MOF crystals
Partial recipeSource: Main

Route 2: Other

8 · Methods - Electronic device

Metal precursorspreformed DDA-Cu film
Linker precursorsnot applicable
Solventswater and ethanol for substrate cleaning
Additives30 nm Au interdigital electrodes
Atmospheresubstrates dried with nitrogen; I-V measured in N2
Temperatureroom temperature measurement
Timenot applicable
Substrate orientationSiO2/Si with 300 nm SiO2; PET for flexible devices
Oxidant / reductantnone
Work-upfilm transferred to substrates coated with interdigital electrodes
Activationsubstrates cleaned by immersion in water and ethanol and dried with nitrogen
Scalability contextdevice geometry reported; transfer protocol sparse
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherDDA-Cu film12 h growth film for I-V tests · about 8 nm thick8 · Methods - Electronic device
OtherSiO2/Si substrate300 nm SiO28 · Methods - Electronic device
OtherAu electrodes30 nm8 · Methods - Electronic device
Solventwater and ethanolnot reported · cleaning8 · Methods - Electronic device
Complete recipeSource: Main

Route 3: Other

8 · Methods - Electrochemical measurement

Metal precursorspre-synthesised DDA-Cu crystals
Linker precursorsnot applicable
Solventsnot specified in main electrode recipe
AdditivesPTFE and conductive carbon black
Atmospherenot reported
Temperature90
Time8
Substrate orientationcoated on nickel foam
Oxidant / reductantnone
Work-upmixed and ground into jelly; coated on 1 x 1 cm nickel foams
Activationdried at 90 C for 8 h and fully dried
Scalability contextabout 4 mg active material for one single electrode
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherDDA-Cu crystalsmass ratio 7; about 4 mg active material8 · Methods - Electrochemical measurement
Additivepolytetrafluoroethylenemass ratio 18 · Methods - Electrochemical measurement
Additiveconductive carbon blackmass ratio 28 · Methods - Electrochemical measurement
Othernickel foam1 x 1 cm8 · Methods - Electrochemical measurement
Complete recipeSource: Main

Route 4: Liquid Liquid Interface

7 · Methods - Synthesis of DDA-Cu MOF film

Metal precursors13.5 mg Cu(CH3COO)2·H2O in 100 mL H2O top layer
Linker precursors5.5 mg DDA in 200 mL CH2Cl2 bottom layer
SolventsCH2Cl2 and H2O
Additivesnone reported
Atmosphereambient / not explicitly controlled
Temperaturenot reported
Time72
Substrate orientationfilm formed at liquid-liquid interface and then transferred to target substrate
Oxidant / reductantnone separately added
Work-upstand for 3 days; stable large-area DDA-Cu MOF film forms at interface
Activationnot reported
Scalability contextstable large-area film reported
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerDDA5.5 mg · 200 mL CH2Cl27 · Methods - Synthesis of DDA-Cu MOF film
Metal SourceCu(CH3COO)2·H2O13.5 mg · 100 mL H2O7 · Methods - Synthesis of DDA-Cu MOF film
SolventCH2Cl2200 mL · bottom layer7 · Methods - Synthesis of DDA-Cu MOF film
SolventH2O100 mL · top layer7 · Methods - Synthesis of DDA-Cu MOF film