cMOF Evidence Base

Synthesis evidence

Intrinsically Conductive π-d Conjugated Layers with Co–N4 Active Sites for Efficient Nitrate Electrocatalysis and Zinc-Nitrate Batteries

Namvar S., Arzani M., Sarkar A.M. et al. · ACS Applied Materials and Interfaces · 2026 · 24433-24443

4 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

p.24436 · Results and Discussion

Metal precursorsPreformed Co3(HITP)2 powder
SolventsIsopropyl alcohol (IPA), 15 mL
AtmosphereNot specified; ambient drying implied.
Time0.5 sonication
Substrate orientationCarbon paper exposed electrode area about 0.25-0.36 cm2
Work-upCatalyst ink drop-cast onto carbon paper until mass loading of about 0.5 mg cm-2.
Scalability contextSmall-area drop-cast electrode; no scale-up method reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo3(HITP)2 powder10-15 mgp.24436 · Results and Discussion
Solventisopropyl alcohol (IPA)15 mLp.24436 · Results and Discussion
Othercarbon paperabout 0.25-0.36 cm2 exposed areap.24436 · Results and Discussion
Complete recipeSource: Both

Route 2: Other

p.24435 · Experimental Section · Figure S1

Metal precursorsCobalt(II) chloride hexahydrate, 0.1 M aqueous solution, 20 mL
Linker precursorsHITP.6HCl, 0.24 mmol in 40 mL distilled water
SolventsDistilled water; water and ethanol washes in main text; SI schematic visually indicates water and IPA washing.
Additives1.2 mL concentrated aqueous ammonia solution (14 M)
AtmosphereNot explicitly specified; aqueous stirring presumed under ambient atmosphere.
Temperature60 drying
Time3 stirring; overnight drying in main text; 24 drying in SI schematic
Oxidant / reductantAqueous ammonia base/coordination promoter
Work-upBlack solid recovered by centrifugation, washed with water and ethanol according to main text; SI schematic shows water and IPA washing.
ActivationDried under vacuum at 60 degC overnight; SI schematic labels 24 h, 60 degC vacuum drying.
Scalability contextBatch aqueous synthesis using 60 mL total precursor solution plus ammonia; no scale-up data reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecobalt(II) chloride hexahydrate20 mL · 0.1 Mp.24435 · Experimental Section · Figure S1
LinkerHITP.6HCl0.24 mmol in 40 mL distilled waterp.24435 · Experimental Section · Figure S1
Solventdistilled water20 mL + 40 mLp.24435 · Experimental Section · Figure S1
Baseconcentrated aqueous ammonia solution1.2 mL · 14 Mp.24435 · Experimental Section · Figure S1
Solventwaterwash solventp.24435 · Experimental Section · Figure S1
Solventethanol; SI schematic visually labels IPAwash solventp.24435 · Experimental Section · Figure S1
Complete recipeSource: SI

Route 3: Drop Cast

S8 · In-Situ ATR-SEIRAS · Figure S10

Metal precursorsPreformed Co3(HITP)2 powder; KAuCl4.2H2O for Au@Si substrate
SolventsIsopropanol for catalyst ink; Milli-Q water, ethanol and acetone substrate sonication solvents
Additives5 wt% Nafion binder; NH4F, HF, Na2SO3, Na2SO3.5H2O and NH4Cl for electroless gold deposition
AtmosphereQuiescent conditions for gold deposition; ambient drying for catalyst film.
Temperatureambient drying
Time1 sonication for catalyst suspension
Substrate orientationUndoped Si(100) ATR FAC prism with nanostructured Au film; geometric exposed Au area 0.71 cm2
Oxidant / reductantElectroless Au deposition solution containing KAuCl4.2H2O and sulfite salts
Work-upSi prism mechanically polished, sonicated 10 min each in Milli-Q water, ethanol and acetone, immersed in 40% NH4F for 3 min, then plated to about 50 nm Au; Co3(HITP)2/Nafion ink dropped onto Au@Si and dried.
Scalability contextSpecialised SEIRAS substrate and electrochemical cell preparation; intended for mechanistic spectroscopy, not bulk catalyst scale-up.
Show 10 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo3(HITP)25 mg mL-1 in isopropanolS8 · In-Situ ATR-SEIRAS · Figure S10
SolventisopropanolNot specifiedS8 · In-Situ ATR-SEIRAS · Figure S10
AdditiveNafion5 wt%S8 · In-Situ ATR-SEIRAS · Figure S10
OtherSi(100) ATR FAC prismNot specifiedS8 · In-Situ ATR-SEIRAS · Figure S10
Acidaqueous NH4F3 min immersion · 40%S8 · In-Situ ATR-SEIRAS · Figure S10
Metal SourceKAuCl4.2H2O0.015 MS8 · In-Situ ATR-SEIRAS · Figure S10
AcidHF2%S8 · In-Situ ATR-SEIRAS · Figure S10
ReductantNa2SO30.15 MS8 · In-Situ ATR-SEIRAS · Figure S10
ReductantNa2SO3.5H2O0.05 MS8 · In-Situ ATR-SEIRAS · Figure S10
AdditiveNH4Cl0.05 MS8 · In-Situ ATR-SEIRAS · Figure S10
Complete recipeSource: SI

Route 4: Other

S10 · Assembly of the zinc-nitrate battery

Metal precursorsPreformed Co3(HITP)2-coated carbon paper cathode; zinc plate anode
SolventsAqueous KNO3/KOH electrolytes
AdditivesNafion 115 proton exchange membrane
AtmosphereNot specified.
Substrate orientationCathode 0.5 x 0.5 cm2; zinc plate 1 x 2 cm2
Oxidant / reductantZinc anode and nitrate catholyte in alkaline battery configuration
Work-upAssembled H-type cell with 10 mL catholyte (1 M KNO3 + 1 M KOH) and 10 mL anolyte (5 M KOH) separated by Nafion 115.
Scalability contextBench H-type battery cell; no stack or large-area assembly reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherCo3(HITP)2-coated carbon paper0.5 x 0.5 cm2S10 · Assembly of the zinc-nitrate battery
Metal Sourcezinc plate1 x 2 cm2S10 · Assembly of the zinc-nitrate battery
ElectrolyteKNO3 + KOH catholyte10 mL · 1 M KNO3 + 1 M KOHS10 · Assembly of the zinc-nitrate battery
ElectrolyteKOH anolyte10 mL · 5 M KOHS10 · Assembly of the zinc-nitrate battery
OtherNafion 115 proton exchange membraneNot specifiedS10 · Assembly of the zinc-nitrate battery