cMOF Evidence Base

Synthesis evidence

Promoting ethylene production over a wide potential window on Cu crystallites induced and stabilized via current shock and charge delocalization

Sun H., Chen L., Xiong L. et al. · Nature Communications · 2021 · 6823

9 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32

Metal precursorsCu3(HHTP)2 powder
SolventsEthanol
AdditivesNafion solution; no Ketjen Black for stand-alone comparison, exact no-KB ink composition not separately specified
AtmosphereRoom temperature drying; atmosphere not specified
Temperatureroom temperature
Substrate orientationGlassy carbon electrode, area 0.197 cm2 in general H-cell recipe
Work-upInk drop-coated and dried at room temperature; exact no-KB ink composition not separately stated
ActivationRepeated cyclic voltammetry from -0.5 to -1.8 V at 10 mV s-1 for 20 min before electrochemical measurement
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 sample powder4 mg implied by general ink recipe8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
AdditiveNafion solution50 uL implied by general ink recipe · 5%8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
Solventethanol1 mL implied by general ink recipe8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
Complete recipeSource: Main

Route 2: Hydrothermal

9 · Methods - Synthesis of Cu3(HHTP)2

Metal precursorsCu(C2H3O2)2
Linker precursorsHHTP
SolventsDI water and DMF
AtmosphereCapped vial; atmosphere not otherwise specified
Temperature80
Time6
Work-upCentrifuged, washed with large amounts of water and ethanol, dried under vacuum
ActivationDried under vacuum
Scalability contextSmall capped-vial synthesis.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(C2H3O2)228.3 mg (0.156 mmol)9 · Methods - Synthesis of Cu3(HHTP)2
LinkerHHTP14 mg (0.044 mmol)9 · Methods - Synthesis of Cu3(HHTP)2
SolventDI water3 mL9 · Methods - Synthesis of Cu3(HHTP)2
SolventDMF0.3 mL added dropwise9 · Methods - Synthesis of Cu3(HHTP)2
Partial recipeSource: Main

Route 3: Other

9 · Methods - Electrochemical measurements

Metal precursorsCu3(HITP)2 catalyst dispersion
SolventsEthanol
Substrate orientationGas diffusion electrode YLS-30T; catalyst-coated side faced electrolyte
Work-upSpray-coated using electric airbrush to 0.8 mg cm-2 loading
Scalability contextFlow cell used 2 x 0.5 cm2 silicone gasket window.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HITP)2 catalyst dispersed in ethanol0.8 mg cm-2 loading9 · Methods - Electrochemical measurements
SolventethanolNot specified9 · Methods - Electrochemical measurements
Partial recipeSource: Main

Route 4: Drop Cast

2, 9 · CO2RR of Cu3(HITP)2 with or without KB; Methods - Electrochemical measurements · Fig. 2

Metal precursorsCu3(HITP)2 powder
SolventsEthanol
AdditivesNafion solution; no Ketjen Black for the stand-alone comparison, but the no-KB ink composition is not separately specified
AtmosphereRoom temperature drying; atmosphere not specified
Temperatureroom temperature
Substrate orientationGlassy carbon electrode, area 0.197 cm2
Work-upInk drop-coated and dried at room temperature; exact no-KB ink composition not separately stated
ActivationRepeated cyclic voltammetry from -0.5 to -1.8 V at 10 mV s-1 for 20 min before electrochemical measurement
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HITP)2 sample powder4 mg implied by general ink recipe2, 9 · CO2RR of Cu3(HITP)2 with or without KB; Methods - Electrochemical measurements · Fig. 2
AdditiveNafion solution50 uL in general ink recipe · 5%2, 9 · CO2RR of Cu3(HITP)2 with or without KB; Methods - Electrochemical measurements · Fig. 2
Solventethanol1 mL in general ink recipe2, 9 · CO2RR of Cu3(HITP)2 with or without KB; Methods - Electrochemical measurements · Fig. 2
Complete recipeSource: Main

Route 5: Other

9 · Methods - Synthesis of Cu3(HITP)2

Metal precursorsCuSO4.5H2O
Linker precursorsHATP.6HCl
SolventsDMA and water
Additives2 M sodium acetate aqueous solution
AtmosphereOpen glass vial; atmosphere not otherwise specified
Temperature65
Time2
Work-upFiltered, washed with large amounts of water and methanol, dried under vacuum
ActivationDried under vacuum
Scalability contextSmall-batch open-vial synthesis in a 50 mL glass vial.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O7 mg (0.028 mmol)9 · Methods - Synthesis of Cu3(HITP)2
LinkerHATP.6HCl10 mg (0.0186 mmol) · in 3 mL water9 · Methods - Synthesis of Cu3(HITP)2
SolventDMA3 mL9 · Methods - Synthesis of Cu3(HITP)2
Solventwater3 mL for linker solution9 · Methods - Synthesis of Cu3(HITP)2
BaseC2H3O2Na aqueous solution4 mL · 2 M9 · Methods - Synthesis of Cu3(HITP)2
Partial recipeSource: Main

Route 6: Drop Cast

8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32

Metal precursorsCu3(HHTP)2 powder
SolventsEthanol
AdditivesKetjen Black and Nafion solution by analogy to general H-cell ink preparation
AtmosphereRoom temperature drying; atmosphere not specified
Temperatureroom temperature
Substrate orientationGlassy carbon electrode, area 0.197 cm2 in general H-cell recipe
Work-upUltrasonic dispersion for 15 min, 10 uL ink drop-coated and dried at room temperature
ActivationRepeated cyclic voltammetry from -0.5 to -1.8 V at 10 mV s-1 for 20 min before electrochemical measurement
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherCu3(HHTP)2 sample powder4 mg implied by general ink recipe8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
AdditiveKetjen Black1 mg implied by general ink recipe8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
AdditiveNafion solution50 uL implied by general ink recipe · 5%8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
Solventethanol1 mL implied by general ink recipe8-9 · Universality of the observations; Methods - Electrochemical measurements · Supplementary Fig. 32
Partial recipeSource: Main

Route 7: Other

9 · Methods - Electrochemical measurements

Metal precursorsKB@Cu3(HITP)2 catalyst dispersion
SolventsEthanol
Substrate orientationGas diffusion electrode YLS-30T; catalyst-coated side faced electrolyte
Work-upSpray-coated using electric airbrush to 0.8 mg cm-2 loading
Scalability contextFlow cell used 2 x 0.5 cm2 silicone gasket window.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercatalyst dispersed in ethanol0.8 mg cm-2 loading9 · Methods - Electrochemical measurements
SolventethanolNot specified9 · Methods - Electrochemical measurements
Complete recipeSource: Main

Route 8: Drop Cast

9 · Methods - Electrochemical measurements

Metal precursorsCu3(HITP)2 powder
SolventsEthanol
AdditivesKetjen Black and 5% Nafion solution
AtmosphereRoom temperature drying; atmosphere not specified
Temperatureroom temperature
Substrate orientationGlassy carbon electrode, area 0.197 cm2
Work-upUltrasonic dispersion for 15 min, 10 uL ink drop-coated and dried at room temperature
ActivationRepeated cyclic voltammetry from -0.5 to -1.8 V at 10 mV s-1 for 20 min before electrochemical measurement
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othersample powder4 mg9 · Methods - Electrochemical measurements
AdditiveKetjen Black1 mg9 · Methods - Electrochemical measurements
AdditiveNafion solution50 uL · 5%9 · Methods - Electrochemical measurements
Solventethanol1 mL9 · Methods - Electrochemical measurements
Partial recipeSource: Main

Route 9: Other

6 · Control studies with naked Cu nanoparticles

Metal precursorsCommercial Cu nanoparticles, 10-30 nm
AdditivesKetjen Black
Substrate orientationH-cell electrode
Work-upMixed with KB; detailed dispersion recipe not separately specified beyond general electrode preparation
ActivationH-cell activation as described for electrochemical measurements
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecommercial Cu nanoparticles10-30 nm6 · Control studies with naked Cu nanoparticles
AdditiveKetjen BlackNot specified6 · Control studies with naked Cu nanoparticles