cMOF Evidence Base

Synthesis evidence

Tunable Carrier Type of a Semiconducting 2D Metal-Organic Framework Cu3(HHTP)2

De Lourdes Gonzalez-Juarez M., Morales C., Flege J.I. et al. · ACS Applied Materials and Interfaces · 2022 · 12404-12411

5 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Electrochemical

SI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2

Metal precursors0.01 M CuSO4 solution electrodeposited as Cu on Au/SiO2 before anodic dissolution.
Linker precursors2.5 mM HHTP in EtOH:H2O solution.
SolventsEtOH:H2O 80:20 for MOF anodic dissolution step; Milli-Q water for solutions.
Additives0.1 M KCl supporting electrolyte for Cu electrodeposition; 0.02 M MTBS supporting electrolyte for MOF anodic dissolution.
AtmosphereCu electrodeposition solution degassed with argon for 10 min; atmosphere during anodic dissolution not further specified.
Temperaturenot specified; apparent room temperature
Time1 h Cu electrodeposition; 2 h anodic dissolution
Substrate orientationAu/SiO2 substrates, 10 x 20 mm, used as working electrodes; Cu layer area 1 cm2 in main text.
Oxidant / reductant-0.270 V for Cu electrodeposition; +0.435 V for anodic dissolution vs standard calomel electrode.
Work-upFilm left on Au/SiO2 for pristine characterisation or subsequently transferred with polymer support.
Scalability contextElectrode area was 1 cm2 in the main text; no larger-scale synthesis described.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper(II) sulfate pentahydrate / CuSO40.01 MSI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2
Electrolytepotassium chloride (KCl)0.1 MSI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2
Linker2,3,6,7,10,11-hexahydroxytriphenylene hydrate (HHTP)2.5 mMSI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2
Electrolytetributylmethylammonium methyl sulfate (MTBS)0.02 MSI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2
SolventEtOH:H2O80:20 solvent ratioSI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2
OtherAu/SiO2 substrate10 x 20 mmSI pp.S1-S2 · Electrochemical deposition of Cu3(HHTP)2 onto Au/SiO2
Complete recipeSource: SI

Route 2: Drop Cast

SI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5

Metal precursorsElectrodeposited Cu3(HHTP)2 film from route_electrodeposited_cuhhtp_on_au_sio2.
SolventsMethanol.
AdditivesPolyacrylic acid transfer support.
Atmospherenot specified
Temperature40
TimePAA solution stirred overnight at room temperature; film dried at 40 C before transfer.
Substrate orientationPAA/MeOH drop-cast onto electrodeposited Cu3(HHTP)2 film.
Work-upTransferred using the same methodology as PMMA.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Additivepolyacrylic acid powder (MW 1800 g/mol)700 mg · 700 mg in 0.3 mL methanolSI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5
Solventmethanol0.3 mLSI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5
Otherelectrodeposited Cu3(HHTP)2 filmNot specifiedSI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5
Complete recipeSource: SI

Route 3: Drop Cast

SI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5

Metal precursorsElectrodeposited Cu3(HHTP)2 film from route_electrodeposited_cuhhtp_on_au_sio2.
SolventsMethanol.
AdditivesPolyacrylic acid transfer support.
Atmospherenot specified
Temperature70
TimePAA solution stirred overnight at room temperature; film dried at 70 C before transfer.
Substrate orientationPAA/MeOH drop-cast onto electrodeposited Cu3(HHTP)2 film.
Work-upTransferred using the same methodology as PMMA.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Additivepolyacrylic acid powder (MW 1800 g/mol)700 mg · 700 mg in 0.3 mL methanolSI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5
Solventmethanol0.3 mLSI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5
Otherelectrodeposited Cu3(HHTP)2 filmNot specifiedSI p.S7 · Cu3(HHTP)2 thin films transferred with PAA · Figure S5
Complete recipeSource: Both

Route 4: Drop Cast

SI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA

Metal precursorsElectrodeposited Cu3(HHTP)2 film from route_electrodeposited_cuhhtp_on_au_sio2.
SolventsChlorobenzene.
AdditivesPoly(methyl methacrylate) transfer support.
Atmospherenot specified
Temperature40
Timeovernight
Substrate orientationPMMA suspension drop-cast onto Cu3(HHTP)2/Au/SiO2 film.
Work-upPMMA/Cu3(HHTP)2 carefully peeled from Au/SiO2 substrate.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Additivepoly(methyl methacrylate) (PMMA)3.71 g · 3.71 g in 10 mL chlorobenzeneSI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA
Solventchlorobenzene10 mLSI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA
Otherelectrodeposited Cu3(HHTP)2 filmNot specifiedSI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA
Complete recipeSource: Both

Route 5: Drop Cast

SI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA

Metal precursorsElectrodeposited Cu3(HHTP)2 film from route_electrodeposited_cuhhtp_on_au_sio2.
SolventsChlorobenzene.
AdditivesPoly(methyl methacrylate) transfer support.
Atmospherenot specified
Temperature70
Timeovernight
Substrate orientationPMMA suspension drop-cast onto Cu3(HHTP)2/Au/SiO2 film.
Work-upPMMA/Cu3(HHTP)2 carefully peeled from Au/SiO2 substrate.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Additivepoly(methyl methacrylate) (PMMA)3.71 g · 3.71 g in 10 mL chlorobenzeneSI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA
Solventchlorobenzene10 mLSI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA
Otherelectrodeposited Cu3(HHTP)2 filmNot specifiedSI p.S2 · Cu3(HHTP)2 thin films transferred with PMMA