Synthesis evidence

Engineering the modulation of the active sites and pores of pristine metal-organic frameworks for high-performance sodium-ion storage

Shuang W., Wang Y., Chen F. et al. · Inorganic Chemistry Frontiers · 2022 · 396-405

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

397 · Preparation of Ni-HHTP-250

Metal precursorsas-prepared Ni-HHTP MOF
Linker precursorsas-prepared Ni-HHTP MOF
Atmosphereargon
Temperature160
Time2
Work-upthermal treatment under Ar; ramp rate 5 C min-1 inferred same as 250 C route
Activationannealing at 160 C
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheras-prepared Ni-HHTP MOFNot specified397 · Preparation of Ni-HHTP-250
Partial recipeSource: Main

Route 2: Other

397 · Preparation of Ni-HHTP-250

Metal precursorsas-prepared Ni-HHTP MOF
Linker precursorsas-prepared Ni-HHTP MOF
Atmosphereargon
Temperature250
Time2
Work-upannealed under argon at 5 C min-1
Activationthermal treatment below carbonisation temperature to remove H2O/OH and expose pores
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheras-prepared Ni-HHTP MOFNot specified397 · Preparation of Ni-HHTP-250
Complete recipeSource: Main

Route 3: Drop Cast

397 · Electrochemical measurements

Metal precursorsNi-HHTP-250 active material
Linker precursorsNi-HHTP-250 active material
SolventsN-methyl-2-pyrrolidone (NMP)
AdditivesKetjen black (20 wt%); polyvinylidene fluoride (PVDF, 10 wt%)
Atmospherevacuum drying; coin cells assembled in Ar glovebox with H2O and O2 <0.5 ppm
Temperature110
Time12
Substrate orientationCu foil current collector
Work-upslurry coated on Cu foil and dried in a vacuum oven
Activationnone beyond vacuum drying
Scalability contextStandard slurry-cast coin-cell electrode; mass loading about 0.8-1.2 mg cm-2.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-HHTP-250 active material70 wt%397 · Electrochemical measurements
AdditiveKetjen black (KB)20 wt%397 · Electrochemical measurements
Additivepolyvinylidene fluoride (PVDF)10 wt%397 · Electrochemical measurements
SolventN-methyl-2-pyrrolidone (NMP)Not specified397 · Electrochemical measurements
Electrolyte1 M NaClO4 in ethylene carbonate/diethyl carbonate (1:1 v/v)1 M397 · Electrochemical measurements
Partial recipeSource: Main

Route 4: Other

397 · Preparation of Ni-HHTP-250

Metal precursorsas-prepared Ni-HHTP MOF
Linker precursorsas-prepared Ni-HHTP MOF
Atmosphereargon
Temperature340
Time2
Work-upthermal treatment under Ar; ramp rate 5 C min-1 inferred same as 250 C route
Activationannealing at 340 C
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheras-prepared Ni-HHTP MOFNot specified397 · Preparation of Ni-HHTP-250
Partial recipeSource: Main

Route 5: Other

397 · Preparation of Ni-HHTP-250

Metal precursorsas-prepared Ni-HHTP MOF
Linker precursorsas-prepared Ni-HHTP MOF
Atmosphereargon
Temperature500
Time2
Work-upthermal treatment under Ar; ramp rate 5 C min-1 inferred same as 250 C route
Activationheating at carbonisation-temperature comparison condition
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otheras-prepared Ni-HHTP MOFNot specified397 · Preparation of Ni-HHTP-250
Partial recipeSource: Main

Route 6: Hydrothermal

397 · Synthesis and characterization · Fig. 1

Metal precursorsnickel acetate tetrahydrate (Ni(OAc)2.4H2O); amount not reported in main text
Linker precursors2,3,6,7,10,11-hexahydroxytriphenylene (HHTP); amount not reported in main text
Solventsnot specified in main text
Additivesnot specified in main text
Atmospherenot specified
Temperature85
Time12
Work-upnot specified in main text
Activationnot specified in main text
Scalability contextMain text cites a previously reported method and does not give reagent amounts, solvent or workup.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel acetate tetrahydrate (Ni(OAc)2.4H2O)Not specified397 · Synthesis and characterization · Fig. 1
Linker2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)Not specified397 · Synthesis and characterization · Fig. 1