Synthesis evidence

From Low-to High-Crystallinity Bimetal-Organic Framework Nanosheet with Highly Exposed Boundaries: An Efficient and Stable Electrocatalyst for Oxygen Evolution Reaction

Xu J., Zhu X., Jia X. · ACS Sustainable Chemistry and Engineering · 2019 · 16629-16639

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: Solvothermal

3 · Material Synthesis

Metal precursors0.375 mmol CoCl2.6H2O and 0.375 mmol FeCl2.4H2O; same raw materials ratio as two-step route
Linker precursors0.75 mmol benzenedicarboxylic acid (BDC)
Solvents32 mL DMF, 2 mL ethanol, 2 mL deionized water
Additives0.8 mL triethylamine (TEA)
Atmospherenot reported
Temperature140
Time48
Work-upNot separately stated; inferred same collection/wash/freeze-dry workup as main CoFe-MOF route.
ActivationNo separate activation reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMF/ethanol/deionized water32 mL / 2 mL / 2 mL3 · Material Synthesis
LinkerBDC0.75 mmol3 · Material Synthesis
Metal SourceCoCl2.6H2O0.375 mmol3 · Material Synthesis
Metal SourceFeCl2.4H2O0.375 mmol3 · Material Synthesis
BaseTEA0.8 mL3 · Material Synthesis
Partial recipeSource: Main

Route 2: Other

3 · Material Synthesis

Metal precursors0.375 mmol CoCl2.6H2O and 0.375 mmol FeCl2.4H2O; same raw materials ratio as two-step route
Linker precursors0.75 mmol benzenedicarboxylic acid (BDC)
Solvents32 mL DMF, 2 mL ethanol, 2 mL deionized water
Additives0.8 mL triethylamine (TEA)
Atmospherenot reported
Temperaturenot reported for ultrasonic bath
Time8
Work-upNot separately stated; inferred same collection/wash/freeze-dry workup as main CoFe-MOF route.
ActivationNo separate activation reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMF/ethanol/deionized water32 mL / 2 mL / 2 mL3 · Material Synthesis
LinkerBDC0.75 mmol3 · Material Synthesis
Metal SourceCoCl2.6H2O0.375 mmol3 · Material Synthesis
Metal SourceFeCl2.4H2O0.375 mmol3 · Material Synthesis
BaseTEA0.8 mL3 · Material Synthesis
Partial recipeSource: Main

Route 3: Drop Cast

3 · Electrochemical Characterizations

Solvents0.2 mL ethanol and 0.8 mL deionized water
Additives50 uL 5% Nafion
Atmosphereambient drying, not otherwise reported
Temperatureroom temperature
Timesonication >0.5 h; drying 0.25 h
Substrate orientationprepolished glassy carbon electrode, 3 mm diameter
Work-up5 uL ink cast onto GCE and dried for 15 min.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-obtained MOF powders5 mg3 · Electrochemical Characterizations
Solventethanol0.2 mL3 · Electrochemical Characterizations
Solventdeionized water0.8 mL3 · Electrochemical Characterizations
AdditiveNafion50 uL · 5%3 · Electrochemical Characterizations
Partial recipeSource: Main

Route 4: Solvothermal

3 · Material Synthesis

Metal precursors0.375 mmol CoCl2.6H2O and 0.375 mmol FeCl2.4H2O
Linker precursors0.75 mmol benzenedicarboxylic acid (BDC)
Solvents32 mL N,N-dimethylformamide (DMF), 2 mL ethanol, 2 mL deionized water
Additives0.8 mL triethylamine (TEA)
Atmospherenot reported
Temperature140
Time8 h ultrasonic reaction plus 48 h solvothermal treatment
Work-upCooled to room temperature, centrifuged, washed with ethanol and deionized water three times.
ActivationFreeze-dried for 24 h; no separate evacuation/thermal activation reported.
Scalability contextBatch process in a 100 mL PTFE tube/pressure bottle; authors describe it as facile and general but do not report scale-up.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
SolventN,N-dimethylformamide (DMF)32 mL3 · Material Synthesis
Solventethanol2 mL3 · Material Synthesis
Solventdeionized water2 mL3 · Material Synthesis
Linkerbenzenedicarboxylic acid (BDC)0.75 mmol3 · Material Synthesis
Metal SourceCoCl2.6H2O0.375 mmol3 · Material Synthesis
Metal SourceFeCl2.4H2O0.375 mmol3 · Material Synthesis
Basetriethylamine (TEA)0.8 mL3 · Material Synthesis