Synthesis evidence

Fabrication of Hierarchical Porous Metal-Organic Framework Electrode for Aqueous Asymmetric Supercapacitor

Gao W., Chen D., Quan H. et al. · ACS Sustainable Chemistry and Engineering · 2017 · 4144-4153

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

p002 · Preparation of HP-UiO-66

Metal precursors0.180 g ZrCl4; 0.223 g Zn(NO3)2
Linker precursors0.160 g H2BDC
Solvents20 mL anhydrous N,N-dimethylformamide (DMF)
AdditivesHydrochloric acid solution, pH = 1.0, used for etching
Atmospherenot reported
Temperature120
Time24
Work-upSonicate 20 min; heat at 120 C for 24 h; cool naturally; centrifuge; wash several times with DMF and acetone; disperse in pH 1.0 HCl and agitate about 10 min; centrifuge; wash several times with DMF and acetone.
ActivationDried at 60 C overnight in an oven.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrCl4 (Alfa Aesar)0.180 gp002 · Preparation of HP-UiO-66
LinkerH2BDC (Aladdin)0.160 gp002 · Preparation of HP-UiO-66
Metal SourceZn(NO3)2 (Alfa Aesar)0.223 gp002 · Preparation of HP-UiO-66
Solventanhydrous N,N-dimethylformamide (DMF, Alfa Aesar)20 mLp002 · Preparation of HP-UiO-66
Acidhydrochloric acid solutionpH = 1.0p002 · Preparation of HP-UiO-66
SolventacetoneNot specifiedp002 · Preparation of HP-UiO-66
Complete recipeSource: Main

Route 2: Drop Cast

p002 · Electrochemical Measurements

SolventsN-methyl-2-pyrrolidone
Additivesconductive carbon black; PVDF binder
Atmospherenot reported
Temperature80
Time12
Substrate orientationclean Ni foam
Work-upActive material, carbon black and PVDF mixed with N-methyl-2-pyrrolidone into slurry; slurry coated on clean Ni foam.
ActivationWorking electrodes dried at 80 C for 12 h.
Scalability contextLoading density of active materials was about 3 mg cm-2.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheractive materials70 wt %p002 · Electrochemical Measurements
Additiveconductive carbon black20 wt %p002 · Electrochemical Measurements
Additivepolyvinylidene fluoride (PVDF)10 wt %p002 · Electrochemical Measurements
SolventN-methyl-2-pyrrolidoneNot specifiedp002 · Electrochemical Measurements
Complete recipeSource: Main

Route 3: Other

p002 · Electrochemical Measurements

Solvents6 M KOH aqueous electrolyte
Additivespolypropylene membrane separator
Atmosphereambient, not otherwise reported
Temperature20
Substrate orientationtwo stacked working electrodes
Work-upHP-UiO-66 and biomass-derived porous carbon used as positive and negative electrodes; two working electrodes stacked and separated by polypropylene membrane.
Scalability contextHP-UiO-66 loading 2.8 mg; porous carbon loading 2.9 mg; total loading 5.7 mg; mass ratio about 0.96.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherHP-UiO-66 electrode2.8 mgp002 · Electrochemical Measurements
Otherbiomass-derived porous carbon electrode2.9 mgp002 · Electrochemical Measurements
ElectrolyteKOH aqueous solution6 Mp002 · Electrochemical Measurements
Otherpolypropylene membraneNot specifiedp002 · Electrochemical Measurements
Complete recipeSource: Main

Route 4: Solvothermal

p002 · Preparation of HP-UiO-66

Metal precursorsZrCl4; same process as HP-UiO-66 but without Zn(NO3)2
Linker precursorsH2BDC
SolventsAnhydrous N,N-dimethylformamide (DMF)
Additivesnone reported
Atmospherenot reported
Temperature120
Time24
Work-upPrepared by the same process as HP-UiO-66 without Zn(NO3)2 and without acid etching; washed with DMF and acetone.
ActivationDried at 60 C overnight in an oven by the same process.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrCl4same as HP-UiO-66 route; likely 0.180 gp002 · Preparation of HP-UiO-66
LinkerH2BDCsame as HP-UiO-66 route; likely 0.160 gp002 · Preparation of HP-UiO-66
Solventanhydrous N,N-dimethylformamide (DMF)same as HP-UiO-66 route; likely 20 mLp002 · Preparation of HP-UiO-66
SolventacetoneNot specifiedp002 · Preparation of HP-UiO-66