Synthesis evidence

Encapsulating metal organic framework into hollow mesoporous carbon sphere as efficient oxygen bifunctional electrocatalyst

Xiong W., Li H., You H. et al. · National Science Review · 2020 · 609-619

9 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

617 · Preparation of Co-HMCS

Metal precursorsCo(NO3)2 methanol solution
Linker precursorsnone
Solventsmethanol
AdditivesHMCS
Temperature5 C bath
Time30 min ultrasonic dispersion; overnight shaking; 24 h at 5 C
Work-upCentrifuged and washed several times until supernatant was colourless
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
AdditiveHMCS10 mg617 · Preparation of Co-HMCS
Metal SourceCo(NO3)2 methanol solution4 mL · 10 mg mL^-1617 · Preparation of Co-HMCS
SolventmethanolNot specified617 · Preparation of Co-HMCS
Complete recipeSource: Main

Route 2: Other

616 · Preparation of the HMCS

Solvents140 mL ethanol; 20 mL H2O; 320 mL aqueous dopamine solution
Additives6 mL NH4OH; TEOS silica precursor; dopamine carbon source; NaOH etchant
Atmospherenitrogen during calcination
Temperature800 C calcination; 70 C etch
Time0.5 h TEOS reaction; 12 h dopamine reaction; 5 h calcination; 24 h etch
Work-upCentrifuged, washed several times with water and ethanol, dried; etched with 1 M NaOH
ActivationCalcined at 800 C for 5 h under nitrogen
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
BaseNH4OH6 mL · 25-28 wt%616 · Preparation of the HMCS
Solventethanol140 mL616 · Preparation of the HMCS
SolventH2O20 mL616 · Preparation of the HMCS
OtherTEOS5.6 mL · 99%616 · Preparation of the HMCS
Otherdopamine aqueous solution320 mL · 2.5 mg mL^-1616 · Preparation of the HMCS
BaseNaOH1 M616 · Preparation of the HMCS
Complete recipeSource: Main

Route 3: Other

616 · Preparation of the HMCS

SolventsAs HMCS route
AdditivesDopamine concentration increased to 5.0 mg mL^-1
Atmospherenitrogen during calcination
Temperature800 C calcination; 70 C etch
TimeAs HMCS route
Work-upAs HMCS route
ActivationCalcined at 800 C for 5 h under nitrogen
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otherdopamine aqueous solution320 mL · 5.0 mg mL^-1616 · Preparation of the HMCS
Complete recipeSource: Main

Route 4: Drop Cast

617 · Electrochemical experiments

Solvents1 mL isopropanol
Additives40 uL Nafion solution (5 wt%)
Temperatureroom temperature drying
Time30 min ultrasonic treatment
Substrate orientationglassy carbon disk, 0.197 cm2
Work-up20 uL ink drop-cast and dried at room temperature
ActivationCV conditioning before ORR/OER tests
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Otheras-prepared catalyst2.5 mg617 · Electrochemical experiments
Solventisopropanol1 mL617 · Electrochemical experiments
AdditiveNafion solution40 uL · 5 wt%617 · Electrochemical experiments
Partial recipeSource: Main

Route 5: Other

617 · Preparation of ZIF-67@HMCS

Metal precursorsCo(NO3)2 methanol solution
Linker precursors2-MI methanol solution
Solventsmethanol
Temperature5 C bath
TimeSimilar to ZIF@HMCS route
Work-upCentrifuged and washed
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2 methanol solution10 mg mL^-1617 · Preparation of ZIF-67@HMCS
Linker2-MI methanol solution13.12 mg mL^-1617 · Preparation of ZIF-67@HMCS
Complete recipeSource: Main

Route 6: Other

616-617 · Preparation of ZIF-67@HMCS

Metal precursorsCo(NO3)2 methanol solution
Linker precursors2-MI methanol solution
Solventsmethanol
AdditivesHMCS
Temperature5 C bath
Time2 h ultrasonic treatment; overnight shaking; 24 h at 5 C
Work-upCentrifuged and washed
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
AdditiveHMCS10 mg616-617 · Preparation of ZIF-67@HMCS
Metal SourceCo(NO3)2 methanol solution4 mL · 10 mg mL^-1616-617 · Preparation of ZIF-67@HMCS
Linker2-MI methanol solution4 mL · 13.12 mg mL^-1616-617 · Preparation of ZIF-67@HMCS
Complete recipeSource: Main

Route 7: Other

616 · Preparation of ZIF-67@HMCS

Metal precursorsCo(NO3)2 methanol solution
Linker precursors2-MI methanol solution
Solventsmethanol
AdditivesHMCS-1
Temperature5 C bath
TimeAs ZIF@HMCS route
Work-upCentrifuged and washed
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
AdditiveHMCS-110 mg616 · Preparation of ZIF-67@HMCS
Metal SourceCo(NO3)2 methanol solution4 mL · 10 mg mL^-1616 · Preparation of ZIF-67@HMCS
Linker2-MI methanol solution4 mL · 13.12 mg mL^-1616 · Preparation of ZIF-67@HMCS
Vague recipeSource: Main

Route 8: Other

617 · Preparation of ZIF-67@HMCS

Metal precursorspreformed ZIF-67
Additivespreformed HMCS
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherZIF-67Not specified617 · Preparation of ZIF-67@HMCS
AdditiveHMCSNot specified617 · Preparation of ZIF-67@HMCS
Complete recipeSource: Main

Route 9: Other

616 · Preparation of ZIF-67@HMCS

Metal precursorsCo(NO3)2 methanol solution
Linker precursors2-MI methanol solution
Solventsmethanol
AdditivesHMCS
Temperature5 C bath
Time30 min ultrasonic dispersion; overnight shaking; 24 h at 5 C
Work-upCentrifuged and washed several times until supernatant was colourless
Scalability contextPrepared at 10%, 25% and 50% HMCS:Co(NO3)2.6H2O weight ratios by changing solution volumes.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
AdditiveHMCS10 mg616 · Preparation of ZIF-67@HMCS
Metal SourceCo(NO3)2 methanol solution10 mL, 4 mL or 2 mL · 10 mg mL^-1616 · Preparation of ZIF-67@HMCS
Linker2-MI methanol solution10 mL, 4 mL or 2 mL · 13.12 mg mL^-1616 · Preparation of ZIF-67@HMCS
SolventmethanolNot specified616 · Preparation of ZIF-67@HMCS