cMOF Evidence Base

Synthesis evidence

Fibrous Pb(II)-Based Coordination Polymer Operable as a Photocatalyst and Electrocatalyst for High-Rate, Selective CO2-to-Formate Conversion

Suppaso C., Nakazato R., Nakahata S. et al. · Advanced Functional Materials · 2025 · 2417223

9 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

9 · Experimental Section

Metal precursorsMW_60 KGF-9 sample, 2.5 mg
SolventsDMSO (1 mL)
AdditivesKetjen Black; 5 wt% Nafion solution
Atmospherenot specified during electrode drying
Time1 h hotplate drying after drop-casting
Substrate orientationcarbon paper electrode; coating area 1 cm x 1.5 cm
Work-upSonicated ink 10 min, dropped onto carbon paper, heated on hotplate for 1 h.
ActivationDrying to evaporate solvent.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMW_60 KGF-92.5 mg9 · Experimental Section
AdditiveKetjen Blackvaried from 10 to 40 wt%; optimum 30 wt%9 · Experimental Section
AdditiveNafion solution25 uL optimum; varied 15 to 150 uL · 5 wt%9 · Experimental Section
SolventDMSO1 mL9 · Experimental Section
Complete recipeSource: Main

Route 2: Drop Cast

10 · Experimental Section

Metal precursorsKGF-9, 1.7 mg
Solventsisopropanol (1.0 mL)
AdditivesKB EC600JD, 1.1 mg; 5 wt% Nafion dispersion, 25 uL
Atmospherenot specified during electrode fabrication
Substrate orientationgas diffusion electrode; catalyst area 0.5 cm2; loading 2.4 mg cm-2
Work-upSonicated homogeneous catalyst ink, then applied dropwise in multiple steps onto a GDE.
Scalability contextPrepared for commercial-current-density CO2 electrolysis at 200-300 mA cm-2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherKGF-91.7 mg10 · Experimental Section
AdditiveKB EC600JD1.1 mg10 · Experimental Section
AdditiveNafion dispersion25 uL · 5 wt%10 · Experimental Section
Solventisopropanol1.0 mL10 · Experimental Section
Complete recipeSource: Main

Route 3: Solvothermal

9 · Experimental Section

Metal precursorsPb(NO3)2, 1 mmol in water (20 mL)
Linker precursorsH2tadt, 1 mmol in acetone (20 mL)
Solventswater (20 mL); acetone (20 mL)
Atmosphereclosed vessel; atmosphere not specified
Temperature99.85
Time0.1667
Work-upCollected by filtration; washed several times with deionised water and acetone.
ActivationAllowed to dry naturally at room temperature.
Scalability contextMicrowave route sharply shortens synthesis relative to 48 h ordinary solvothermal route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)21 mmol9 · Experimental Section
LinkerH2tadt1 mmol9 · Experimental Section
Solventwater20 mL9 · Experimental Section
Solventacetone20 mL9 · Experimental Section
Complete recipeSource: Main

Route 4: Solvothermal

9 · Experimental Section

Metal precursorsPb(NO3)2, 1 mmol in water (20 mL)
Linker precursorsH2tadt, 1 mmol in acetone (20 mL)
Solventswater (20 mL); acetone (20 mL)
Atmosphereclosed vessel; atmosphere not specified
Temperature99.85
Time2
Work-upCollected by filtration; washed several times with deionised water and acetone.
ActivationAllowed to dry naturally at room temperature.
Scalability contextMicrowave route sharply shortens synthesis relative to 48 h ordinary solvothermal route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)21 mmol9 · Experimental Section
LinkerH2tadt1 mmol9 · Experimental Section
Solventwater20 mL9 · Experimental Section
Solventacetone20 mL9 · Experimental Section
Complete recipeSource: Main

Route 5: Solvothermal

9 · Experimental Section

Metal precursorsPb(NO3)2, 1 mmol in water (20 mL)
Linker precursorsH2tadt, 1 mmol in acetone (20 mL)
Solventswater (20 mL); acetone (20 mL)
Atmosphereclosed vessel; atmosphere not specified
Temperature99.85
Time0.0333
Work-upCollected by filtration; washed several times with deionised water and acetone.
ActivationAllowed to dry naturally at room temperature.
Scalability contextMicrowave route sharply shortens synthesis relative to 48 h ordinary solvothermal route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)21 mmol9 · Experimental Section
LinkerH2tadt1 mmol9 · Experimental Section
Solventwater20 mL9 · Experimental Section
Solventacetone20 mL9 · Experimental Section
Complete recipeSource: Main

Route 6: Solvothermal

9 · Experimental Section

Metal precursorsPb(NO3)2, 1 mmol in water (20 mL)
Linker precursorsH2tadt, 1 mmol in acetone (20 mL)
Solventswater (20 mL); acetone (20 mL)
Atmosphereclosed vessel; atmosphere not specified
Temperature99.85
Time0.5
Work-upCollected by filtration; washed several times with deionised water and acetone.
ActivationAllowed to dry naturally at room temperature.
Scalability contextMicrowave route sharply shortens synthesis relative to 48 h ordinary solvothermal route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)21 mmol9 · Experimental Section
LinkerH2tadt1 mmol9 · Experimental Section
Solventwater20 mL9 · Experimental Section
Solventacetone20 mL9 · Experimental Section
Complete recipeSource: Main

Route 7: Solvothermal

9 · Experimental Section

Metal precursorsPb(NO3)2, 1 mmol in water (20 mL)
Linker precursorsH2tadt, 1 mmol in acetone (20 mL)
Solventswater (20 mL); acetone (20 mL)
Atmosphereclosed vessel; atmosphere not specified
Temperature99.85
Time1
Work-upCollected by filtration; washed several times with deionised water and acetone.
ActivationAllowed to dry naturally at room temperature.
Scalability contextPhase-pure optimised KGF-9 in 60 min instead of 48 h ordinary solvothermal synthesis.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)21 mmol9 · Experimental Section
LinkerH2tadt1 mmol9 · Experimental Section
Solventwater20 mL9 · Experimental Section
Solventacetone20 mL9 · Experimental Section
Complete recipeSource: Main

Route 8: Solvothermal

9 · Experimental Section

Metal precursorsPb(NO3)2, 1 mmol in water (20 mL)
Linker precursorsH2tadt, 1 mmol in acetone (20 mL)
Solventswater (20 mL); acetone (20 mL)
Atmosphereclosed vessel; atmosphere not specified
Temperature99.85
Time1.5
Work-upCollected by filtration; washed several times with deionised water and acetone.
ActivationAllowed to dry naturally at room temperature.
Scalability contextMicrowave route sharply shortens synthesis relative to 48 h ordinary solvothermal route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)21 mmol9 · Experimental Section
LinkerH2tadt1 mmol9 · Experimental Section
Solventwater20 mL9 · Experimental Section
Solventacetone20 mL9 · Experimental Section
Partial recipeSource: Main

Route 9: Solvothermal

2 · 2.1 Physicochemical Properties

Metal precursorsPb(NO3)2
Linker precursorsH2tadt
Solventsaqueous acetone solution
Atmospherenot specified
Temperature99.85
Time48
Work-upNot fully specified in this paper for ordinary control.
ActivationNot fully specified in this paper for ordinary control.
Scalability contextOrdinary route required 48 h versus 60 min for optimised MW route.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePb(NO3)2Not specified2 · 2.1 Physicochemical Properties
LinkerH2tadtNot specified2 · 2.1 Physicochemical Properties
Solventaqueous acetone solutionNot specified2 · 2.1 Physicochemical Properties