cMOF Evidence Base

Synthesis evidence

Ultrathin metal-organic framework array for efficient electrocatalytic water splitting

Duan J., Chen S., Zhao C. · Nature Communications · 2017 · 15341

8 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Drop Cast

S1 · Supplementary Methods; Synthesis of bulk NiFe-MOF/NF

Metal precursorsBulk NiFe-MOF powder prepared similarly to NiFe-MOF without substrates; initial metal salts not re-listed in SI bulk route.
Linker precursors2,6-naphthalenedicarboxylate ligand by analogy to main NiFe-MOF route
SolventsIsopropanol/water (v/v = 1/3) for electrode ink; aqueous synthesis for powder by analogy
Additives1 wt% Nafion binder
AtmosphereNot specified for powder synthesis; ambient drop-cast
Temperature60 for powder synthesis by analogy; room temperature for drop-cast drying not stated
Time20 for powder synthesis by analogy; drop-cast drying time not stated
Substrate orientationDrop-cast onto nickel foam
Oxidant / reductantNone reported
Work-upPowder dispersed then drop-cast onto NF with loading 0.3 mg cm-2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiFe-MOF powderNot specifiedS1 · Supplementary Methods; Synthesis of bulk NiFe-MOF/NF
Solventisoproponal/waterv/v = 1/3S1 · Supplementary Methods; Synthesis of bulk NiFe-MOF/NF
AdditiveNafion binder1 wt%S1 · Supplementary Methods; Synthesis of bulk NiFe-MOF/NF
Othernickel foam substrateloading 0.3 mg cm-2S1 · Supplementary Methods; Synthesis of bulk NiFe-MOF/NF
Complete recipeSource: SI

Route 2: Other

S1 · Supplementary Methods; Calcination of NiFe-MOF

Metal precursorsPreformed NiFe-MOF
Linker precursorsPreformed NiFe-MOF organic linker residue removed/altered on calcination
SolventsNone
AdditivesNone
AtmosphereN2
Temperature650
Time6
Substrate orientationNot specified
Oxidant / reductantThermal treatment under N2
Work-upCalcination with elevated rate of 5 deg C min-1.
ActivationCalcination is the activation/post-treatment.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otherpreformed NiFe-MOFNot specifiedS1 · Supplementary Methods; Calcination of NiFe-MOF
OtherN2 atmosphereNot specifiedS1 · Supplementary Methods; Calcination of NiFe-MOF
Partial recipeSource: SI

Route 3: Other

S1 · Supplementary Methods; Synthesis of Cu-MOF/NF

Metal precursors10 mg Cu(Ac)2
Linker precursorsSame organic ligand as NiFe-MOF route by reference
SolventsDI-water by reference
AdditivesNickel foam support
AtmosphereSealed vial; not otherwise specified
Temperature60 by reference
Time20 by reference
Substrate orientationNickel foam support immersed
Oxidant / reductantNone reported
Work-upSame as NiFe-MOF/NF by reference; not re-stated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(Ac)210 mgS1 · Supplementary Methods; Synthesis of Cu-MOF/NF
Linker2,6-naphthalenedicarboxylic acid dipotassiumsame as NiFe-MOF/NF by referenceS1 · Supplementary Methods; Synthesis of Cu-MOF/NF
SolventDI-watersame as NiFe-MOF/NF by referenceS1 · Supplementary Methods; Synthesis of Cu-MOF/NF
Othernickel foamsame as NiFe-MOF/NF by referenceS1 · Supplementary Methods; Synthesis of Cu-MOF/NF
Vague recipeSource: Main

Route 4: Other

3 · Electrocatalytic oxygen and hydrogen evolution

Metal precursorsIron salt, likely Fe(NO3)3.9H2O by analogy; exact amount not reported for Fe-only sample
Linker precursors2,6-naphthalenedicarboxylate ligand by analogy
SolventsDI-water by analogy
AdditivesNickel foam support
AtmosphereNot specified
Temperature60 by analogy
Time20 by analogy
Substrate orientationNickel foam support
Oxidant / reductantNone reported
Work-upNot separately reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceiron saltnot specified3 · Electrocatalytic oxygen and hydrogen evolution
Linker2,6-naphthalenedicarboxylatenot specified3 · Electrocatalytic oxygen and hydrogen evolution
Othernickel foam supportNot specified3 · Electrocatalytic oxygen and hydrogen evolution
Vague recipeSource: Main

Route 5: Other

3 · Electrocatalytic oxygen and hydrogen evolution

Metal precursorsNickel salt, likely Ni(Ac)2.4H2O by analogy; exact amount not reported for Ni-only sample
Linker precursors2,6-naphthalenedicarboxylate ligand by analogy
SolventsDI-water by analogy
AdditivesNickel foam support
AtmosphereNot specified
Temperature60 by analogy
Time20 by analogy
Substrate orientationNickel foam support
Oxidant / reductantNone reported
Work-upNot separately reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel saltnot specified3 · Electrocatalytic oxygen and hydrogen evolution
Linker2,6-naphthalenedicarboxylatenot specified3 · Electrocatalytic oxygen and hydrogen evolution
Othernickel foam supportNot specified3 · Electrocatalytic oxygen and hydrogen evolution
Partial recipeSource: SI

Route 6: Drop Cast

S12 · Supplementary Figure 10 · Supplementary Fig. 10

Metal precursorsPreformed NiFe-MOF
Linker precursorsPreformed NiFe-MOF
SolventsNot specified
AdditivesGlassy carbon electrode; binder not stated in caption
AtmosphereAmbient, not specified
Substrate orientationDrop-cast onto glassy carbon
Oxidant / reductantNone reported
Work-upDrop casting with mass loading 0.3 mg cm-2.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Otherpreformed NiFe-MOFloading 0.3 mg cm-2S12 · Supplementary Figure 10 · Supplementary Fig. 10
Otherglassy carbon electrodeNot specifiedS12 · Supplementary Figure 10 · Supplementary Fig. 10
Complete recipeSource: Both

Route 7: Other

6 · Methods; Synthesis of NiFe-MOF electrode

Metal precursors8 mg Ni(Ac)2.4H2O and 2 mg Fe(NO3)3.9H2O
Linker precursors10 mg organic ligand 2,6-naphthalenedicarboxylate tetrahydrate / 2,6-naphthalenedicarboxylic acid dipotassium
Solvents1 mL DI-water
AdditivesNickel foam substrate; no binder
AtmosphereSealed vial; aqueous, atmosphere not otherwise specified
Temperature60
Time20
Substrate orientationNickel foam piece immersed in vial; orientation not specified
Oxidant / reductantNone reported
Work-upCool to room temperature, remove nickel foam, bath ultrasonicate 1 min, rinse with copious DI-water.
ActivationNo separate activation reported before electrocatalysis.
Scalability contextPiece size 2 cm x 1 cm x 1.6 mm; strategy claimed adaptable to other substrates and metals.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(Ac)2.4H2O8 mg6 · Methods; Synthesis of NiFe-MOF electrode
Metal SourceFe(NO3)3.9H2O2 mg6 · Methods; Synthesis of NiFe-MOF electrode
Linker2,6-naphthalenedicarboxylate tetrahydrate / dipotassium10 mg6 · Methods; Synthesis of NiFe-MOF electrode
SolventDI-water1 mL · 18 Mohm cm6 · Methods; Synthesis of NiFe-MOF electrode
Othernickel foam2 cm x 1 cm x 1.6 mm6 · Methods; Synthesis of NiFe-MOF electrode
Partial recipeSource: SI

Route 8: Other

S1 · Supplementary Methods; Synthesis of NiFe-MOF/stainless steel mesh

Metal precursorsSame as NiFe-MOF/NF route by reference
Linker precursorsSame as NiFe-MOF/NF route by reference
SolventsDI-water by reference
AdditivesStainless steel mesh support
AtmosphereSealed vial; not otherwise specified
Temperature60 by reference
Time20 by reference
Substrate orientationStainless steel mesh used as support
Oxidant / reductantNone reported
Work-upSame as NiFe-MOF/NF by reference; not re-stated.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi(Ac)2.4H2Osame as NiFe-MOF/NF by referenceS1 · Supplementary Methods; Synthesis of NiFe-MOF/stainless steel mesh
Metal SourceFe(NO3)3.9H2Osame as NiFe-MOF/NF by referenceS1 · Supplementary Methods; Synthesis of NiFe-MOF/stainless steel mesh
Linker2,6-naphthalenedicarboxylic acid dipotassiumsame as NiFe-MOF/NF by referenceS1 · Supplementary Methods; Synthesis of NiFe-MOF/stainless steel mesh
Otherstainless steel mesh300 mesh; wire diameter 0.04 mmS1 · Supplementary Methods; Synthesis of NiFe-MOF/stainless steel mesh