cMOF Evidence Base

Synthesis evidence

Nanocubic bimetallic organic framework self-templated from Ni precursor as efficient electrocatalysts for oxygen evolution reaction

Yuan B., Li C., Liu Y. et al. · International Journal of Hydrogen Energy · 2019 · 11705-11716

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Solvothermal

11706 · Synthetic section

Metal precursorsferrous chloride (FeCl2.4H2O, 0.3816 g, 1.92 mmol)
Linker precursorsterephthalic acid (C8H6O4, 0.0800 g, 0.48 mmol)
Solventsdistilled water (1 mL), ethanol (1 mL), N,N-dimethylformamide (DMF, 14 mL)
Atmospheresealed Teflon-lined stainless-steel autoclave; atmosphere not otherwise specified
Temperature125
Time12
Work-upStirred 30 min before autoclave; after cooling, brown precipitate collected by centrifugation and washed with mixed deionized water/ethanol several times.
ActivationDried at 60 C overnight.
Scalability context25 mL Teflon-lined autoclave; no yield reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceferrous chloride (FeCl2.4H2O)0.3816 g, 1.92 mmol11706 · Synthetic section
Linkerterephthalic acid (C8H6O4)0.0800 g, 0.48 mmol11706 · Synthetic section
Solventdistilled water1 mL11706 · Synthetic section
Solventethanol1 mL11706 · Synthetic section
SolventN,N-dimethylformamide (DMF)14 mL11706 · Synthetic section
Complete recipeSource: Main

Route 2: Other

11706 · Synthetic section

Metal precursorsnickel acetate tetrahydrate (Ni(CH3COO)2.4H2O, 1.75 g)
Solventsethanol (250 mL)
Additivespolyvinylpyrrolidone (PVP K30, MW about 40000, 3.75 g)
Atmosphereambient; dried in air
Temperature90
Time10
Work-upCentrifuged at least 5 times at 8000 rpm to remove surface-attached PVP.
ActivationCompletely dried in air to obtain precipitate.
Scalability context250 mL ethanol batch in 500 mL round-bottom flask; no yield reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcenickel acetate tetrahydrate (Ni(CH3COO)2.4H2O)1.75 g11706 · Synthetic section
Additivepolyvinyl pyrrolidone (PVP)3.75 g11706 · Synthetic section
Solventethanol250 mL11706 · Synthetic section
Complete recipeSource: Main

Route 3: Solvothermal

11706-11707 · Synthetic section

Metal precursorsobtained Ni NCs (0.2862 g) and ferrous chloride (FeCl2.4H2O, 0.0954 g)
Linker precursorsterephthalic acid (C8H6O4, 0.0800 g)
SolventsDMF (14 mL), ethanol (1 mL), distilled water (1 mL)
AdditivesNi NCs act as template and Ni source
Atmospheresealed Teflon-lined stainless-steel autoclave; atmosphere not otherwise specified
Temperature125
Time12
Oxidant / reductantNo separate oxidant/reductant; Fe2+ hydrolysis/protons release Ni2+ from Ni NCs according to mechanism.
Work-upOther steps same as MIL-53(Fe): stir 30 min, solvothermal treatment, centrifuge, wash with water/ethanol.
ActivationOther steps same as MIL-53(Fe): dried at 60 C overnight.
Scalability context25 mL autoclave inherited from MIL-53(Fe) procedure; no yield reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceobtained Ni NCs0.2862 g11706-11707 · Synthetic section
Metal Sourceferrous chloride (FeCl2.4H2O)0.0954 g11706-11707 · Synthetic section
Linkerterephthalic acid (C8H6O4)0.0800 g11706-11707 · Synthetic section
SolventN,N-dimethylformamide (DMF)14 mL11706-11707 · Synthetic section
Solventethanol1 mL11706-11707 · Synthetic section
Solventdistilled water1 mL11706-11707 · Synthetic section
Partial recipeSource: SI

Route 4: Solvothermal

3/8 · Supporting Information · Fig. S2, Fig. S3

Metal precursorsNi NCs and FeCl2 varied by mass ratio 0.5, 1, 2, 3, 4
Linker precursorsterephthalic acid, amount not repeated in SI captions
Solventsnot repeated in SI captions; assumed same solvent system as main target route
AdditivesNi NCs template
Atmospherenot specified for variants
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNi NCsmass-ratio series versus FeCl2: 0.5, 1, 2, 3, 43/8 · Supporting Information · Fig. S2, Fig. S3
Metal SourceFeCl2mass-ratio series versus Ni NCs: 0.5, 1, 2, 3, 43/8 · Supporting Information · Fig. S2, Fig. S3