cMOF Evidence Base

Synthesis evidence

Single-Site, Single-Metal-Atom, Heterogeneous Electrocatalyst: Metal–Organic-Framework Supported Molybdenum Sulfide for Redox Mediator-Assisted Hydrogen Evolution Reaction

Noh H., Yang Y., Zhang X. et al. · ChemElectroChem · 2020 · 509-516

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

516 · References note 39

Metal precursorsMo(VI) ions / metal precursor in solution-phase SIM
Linker precursorsNDC-SALI/NU-1000 framework
Solventsinert solvent such as heptane described for SIM generally; exact solvent not restated for this sample
Additivesnot restated
Atmospherenot restated; SIM described using inert solvent
Timeovernight typical for SIM according to reference note, exact time not restated
Oxidant / reductantMo(VI) oxide deposition prior to H2S reduction/sulfidation
Work-upextensive washing with solvent to remove uncoordinated metal precursors is described for SIM generally
Activationthermal activation to remove solvent from MOF pores is described for SIM generally
Scalability contextbulk powder postsynthetic metal installation
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMo(VI) ions / metal precursorNot specified516 · References note 39
Solventinert solvent, e.g. heptane (generic SIM description)Not specified516 · References note 39
OtherNDC-SALIbulk MOF powders516 · References note 39
Complete recipeSource: Main

Route 2: Drop Cast

515 · Experimental Section

Metal precursorsMoSx-SIM-NDC-SALI powder
Linker precursorsframework already synthesised
Solventsethanol dried with MgSO4; dried ethanol purged with N2 for sulfide electrodes
Additivespolyamide tape to define electroactive area
Atmospheresulfide-based electrodes prepared in argon-filled glovebox; electrolyte purged with N2 before measurement
Temperatureroom temperature drying implied
Timebrief sonication; dry before use; N2 purge 20 min before sulfide suspension addition and at least 20 min before electrochemical measurement
Substrate orientationFTO substrate; electroactive area 0.25 cm2
Work-up10 mg MOF in 1 mL dried ethanol, briefly sonicated; 3 uL drop-cast onto FTO; once dried used as working electrode
Activationnone beyond drying; after electrolysis headspace gas sampled for GC
Scalability contextsmall-area drop-cast test electrode, not a scalable film-growth process
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherMoSx-SIM-NDC-SALI10 mg · 10 mg in 1 mL ethanol515 · Experimental Section
Solventethanol dried with MgSO41 mL515 · Experimental Section
Additivepolyamide tapeNot specified515 · Experimental Section
OtherFTO substrate0.25 cm2 electroactive area515 · Experimental Section
Partial recipeSource: Both

Route 3: Other

510 · Introduction

Metal precursorsMoOx-SIM-NDC-SALI / Mo(VI)-loaded NDC-SALI
Linker precursorsTBAPy and NDC in NU-1000 framework
Solventsnone stated for gas-phase H2S treatment
AdditivesH2S gas
Atmospheregas-phase H2S at elevated temperature; sulfide material handled in argon-filled glovebox after treatment
Temperatureelevated temperature; exact value not restated
Oxidant / reductantH2S reduces Mo(VI) to Mo(IV) and replaces two oxo ligands by sulfhydryl ligands
Work-upafter H2S treatment, sulfide-based materials brought into argon-filled glovebox; ca. 40 mg mounted for sorption without additional treatment
Activationno additional treatment before sulfide sorption measurement
Scalability contextgas-phase postsynthetic sulfidation of bulk MOF powder
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherMoOx-SIM-NDC-SALINot specified510 · Introduction
ReductantH2Sgas phase510 · Introduction
Partial recipeSource: Main

Route 4: Other

512 · Electrocatalytic Hydrogen Evolution

Metal precursorsMo(VI) ions installed in NU-1000 by solution-phase SIM
Linker precursorsNU-1000 TBAPy framework without NDC
Solventsnot restated; SIM generally uses inert solvent such as heptane
AdditivesH2S gas for sulfidation
Atmospheregas-phase H2S for sulfide conversion; other details in cited previous work
Oxidant / reductantMo(VI) to Mo(IV) reduction by H2S
Work-upnot restated
Activationnot restated
Scalability contextNDC-free comparator made according to prior procedure
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceMo(VI) ions / metal precursorNot specified512 · Electrocatalytic Hydrogen Evolution
ReductantH2Sgas phase512 · Electrocatalytic Hydrogen Evolution
OtherNU-1000Not specified512 · Electrocatalytic Hydrogen Evolution
Partial recipeSource: Main

Route 5: Other

516 · References note 41

Metal precursorsNU-1000 Zr6 nodes
Linker precursorsnaphthalene dicarboxylate (NDC) ligand/site-directing agent
SolventsDMF implied by SALI description in cited procedure; exact solvent/amount not restated
Additivesnot restated
Atmospherenot restated
Work-upSALI generally involves soaking bulk MOF powders in ligand solution; detailed washing not restated
Activationnot restated for synthesis; sorption activation 120 degrees C for 12 h for non-air-sensitive samples
Scalability contextbulk powder postsynthetic ligand incorporation
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkernaphthalene dicarboxylate (NDC)Not specified516 · References note 41
SolventN,N-dimethylformamide (typical SALI solvent, cited)Not specified516 · References note 41
OtherNU-1000bulk MOF powders516 · References note 41
Partial recipeSource: Both

Route 6: Unknown

515 · Experimental Section

Metal precursorsnot restated; Zr precursor in cited NU-1000 procedures
Linker precursorsH4TBAPy linker synthesised as reported previously
Solventsnot restated for NU-1000 synthesis
Additivesnot restated
Atmospherenot restated
Work-upnot restated
ActivationSorption samples not air-sensitive activated at 120 degrees C for 12 h before measurement
Scalability contextbulk MOF powder used for postsynthetic modification
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH4TBAPy linkerNot specified515 · Experimental Section
OtherZr precursor not restated in local paperNot specified515 · Experimental Section