Synthesis evidence

Why conductivity is not always king-physical properties governing the capacitance of 2D metal-organic framework-based EDLC supercapacitor electrodes: A Ni3(HITP)2case study

Borysiewicz M.A., Dou J.-H., Stassen I. et al. · Faraday Discussions · 2021 · 298-304

3 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Solvothermal

SI p.S1 · MOF synthesis

Metal precursorsNickel chloride hexahydrate (NiCl2.6H2O).
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl).
SolventsDeionised water.
AdditivesSodium acetate (CH3COONa) base.
AtmosphereAqueous solution under air at 60 C; 250 ml round-bottom flask bubbled with air for 45 min and then nitrogen for 1.5 h.
Temperature60
Time0.75 h air bubbling plus 1.5 h nitrogen bubbling
Oxidant / reductantAir used during reaction/bubbling; no separate oxidant or reductant specified.
Work-upResulting black powder centrifuged, washed in water and then ethanol, and dried on the Schlenk line for 2 h.
ActivationDried on Schlenk line for 2 h; no separate activation reported.
Scalability context250 ml round-bottom flask; study notes common laboratory settings and batch-to-batch variation rather than scale-up.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel chloride hexahydrate (NiCl2.6 H2O)Not specifiedSI p.S1 · MOF synthesis
Linker2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6 HCl)HATP.6HCl : NiCl2.6H2O = 2:3 molar ratioSI p.S1 · MOF synthesis
SolventDeionised waterNot specifiedSI p.S1 · MOF synthesis
BaseSodium acetate, CH3COONaNot specifiedSI p.S1 · MOF synthesis
Partial recipeSource: Both

Route 2: Solvothermal

SI p.S1 · MOF synthesis

Metal precursorsNickel chloride hexahydrate (NiCl2.6H2O).
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl).
SolventsDeionised water.
Additives14 M ammonia (NH4OH) base.
AtmosphereAqueous solution under air at 60 C; open 250 ml beaker bubbled with air for 2 h.
Temperature60
Time2
Oxidant / reductantAir used during reaction/bubbling; no separate oxidant or reductant specified.
Work-upResulting black powder centrifuged, washed in water and then ethanol, and dried on the Schlenk line for 2 h.
ActivationDried on Schlenk line for 2 h; no separate activation reported.
Scalability contextOpen 250 ml beaker.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel chloride hexahydrate (NiCl2.6 H2O)Not specifiedSI p.S1 · MOF synthesis
Linker2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6 HCl)HATP.6HCl : NiCl2.6H2O = 2:3 molar ratioSI p.S1 · MOF synthesis
SolventDeionised waterNot specifiedSI p.S1 · MOF synthesis
Base14 M ammonia, NH4OH14 MSI p.S1 · MOF synthesis
Partial recipeSource: Both

Route 3: Solvothermal

SI p.S1 · MOF synthesis

Metal precursorsNickel chloride hexahydrate (NiCl2.6H2O).
Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl).
SolventsDeionised water.
Additives14 M ammonia (NH4OH) base.
AtmosphereAqueous solution under air at 60 C; same as HITP_B but in 50 ml beaker.
Temperature60
Time2
Oxidant / reductantAir used during reaction/bubbling; no separate oxidant or reductant specified.
Work-upResulting black powder centrifuged, washed in water and then ethanol, and dried on the Schlenk line for 20 h.
ActivationDried on Schlenk line for 20 h; no separate activation reported.
Scalability contextSmaller scale than HITP_B, using a 50 ml beaker.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel chloride hexahydrate (NiCl2.6 H2O)Not specifiedSI p.S1 · MOF synthesis
Linker2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6 HCl)HATP.6HCl : NiCl2.6H2O = 2:3 molar ratioSI p.S1 · MOF synthesis
SolventDeionised waterNot specifiedSI p.S1 · MOF synthesis
Base14 M ammonia, NH4OH14 MSI p.S1 · MOF synthesis