Synthesis evidence

Unleashing the room temperature boronization: Blooming of Ni-ZIF nanobuds for efficient photo/electro catalysis of water

John G., Priyadarshini S., babu A. et al. · Chemosphere · 2024 · 140574

10 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1

Metal precursors0.05 g pre-synthesised Ni-ZIF
Linker precursorsNi-ZIF framework contains 2-methylimidazolate linker
Solvents25 mL water for NaBH4 solution; DI water and ethanol washing
Additivesnone reported
Atmosphereroom temperature; atmosphere not stated
Temperatureroom temperature for boronization; 80 deg C drying
Time24
Substrate orientationnone; powder immersion
Oxidant / reductantNaBH4 (sodium borohydride), 1 M, reductant and boron source
Work-upResidue taken out and cleaned with DI water and ethanol six times
Activationovernight dried at 80 deg C
Scalability contextBatch powder immersion; no yield or scale-up reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-ZIF0.05 g2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
ReductantNaBH4 (sodium borohydride)25 ml water + 1 M sodium borohydride solution · 1 M2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventwater25 ml2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
SolventDI waterwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventethanolwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Partial recipeSource: Both

Route 2: Drop Cast

3,8 · 2.5 Electrocatalytic measurements; 3.2

Metal precursors24-BNZ active material already synthesised
Linker precursorsin active material
Solventsslurry solvent not stated
Additives10 mg carbon black; 10 mg PVDF binder
Atmospherenot stated
Temperature80
Time24
Substrate orientationNickel foam, electrode area 1 x 1 cm
Oxidant / reductantnone during electrode fabrication
Work-upSlurry drop-cast onto nickel foam substrate
Activationdried for 1 day at 80 deg C; electrochemical activation by 100 CV cycles at 100 mV/s before tests
Scalability contextElectrode ink uses 80 wt% active material, 10 wt% carbon black, 10 wt% PVDF by stated masses; slurry solvent not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Other24-BNZ80 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Additivecarbon black10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
AdditivePVDF (polyvinylidene difluoride)10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Othernickel foam1 x 1 cm working area; 1.5 mm thickness3,8 · 2.5 Electrocatalytic measurements; 3.2
Complete recipeSource: Both

Route 3: Other

2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1

Metal precursors0.05 g pre-synthesised Ni-ZIF
Linker precursorsNi-ZIF framework contains 2-methylimidazolate linker
Solvents25 mL water for NaBH4 solution; DI water and ethanol washing
Additivesnone reported
Atmosphereroom temperature; atmosphere not stated
Temperatureroom temperature for boronization; 80 deg C drying
Time48
Substrate orientationnone; powder immersion
Oxidant / reductantNaBH4 (sodium borohydride), 1 M, reductant and boron source
Work-upResidue taken out and cleaned with DI water and ethanol six times
Activationovernight dried at 80 deg C
Scalability contextBatch powder immersion; no yield or scale-up reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-ZIF0.05 g2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
ReductantNaBH4 (sodium borohydride)25 ml water + 1 M sodium borohydride solution · 1 M2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventwater25 ml2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
SolventDI waterwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventethanolwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Partial recipeSource: Both

Route 4: Drop Cast

3,8 · 2.5 Electrocatalytic measurements; 3.2

Metal precursors48-BNZ active material already synthesised
Linker precursorsin active material
Solventsslurry solvent not stated
Additives10 mg carbon black; 10 mg PVDF binder
Atmospherenot stated
Temperature80
Time24
Substrate orientationNickel foam, electrode area 1 x 1 cm
Oxidant / reductantnone during electrode fabrication
Work-upSlurry drop-cast onto nickel foam substrate
Activationdried for 1 day at 80 deg C; electrochemical activation by 100 CV cycles at 100 mV/s before tests
Scalability contextElectrode ink uses 80 wt% active material, 10 wt% carbon black, 10 wt% PVDF by stated masses; slurry solvent not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Other48-BNZ80 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Additivecarbon black10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
AdditivePVDF (polyvinylidene difluoride)10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Othernickel foam1 x 1 cm working area; 1.5 mm thickness3,8 · 2.5 Electrocatalytic measurements; 3.2
Complete recipeSource: Both

Route 5: Other

2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1

Metal precursors0.05 g pre-synthesised Ni-ZIF
Linker precursorsNi-ZIF framework contains 2-methylimidazolate linker
Solvents25 mL water for NaBH4 solution; DI water and ethanol washing
Additivesnone reported
Atmosphereroom temperature; atmosphere not stated
Temperatureroom temperature for boronization; 80 deg C drying
Time4
Substrate orientationnone; powder immersion
Oxidant / reductantNaBH4 (sodium borohydride), 1 M, reductant and boron source
Work-upResidue taken out and cleaned with DI water and ethanol six times
Activationovernight dried at 80 deg C
Scalability contextBatch powder immersion; no yield or scale-up reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-ZIF0.05 g2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
ReductantNaBH4 (sodium borohydride)25 ml water + 1 M sodium borohydride solution · 1 M2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventwater25 ml2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
SolventDI waterwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventethanolwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Partial recipeSource: Both

Route 6: Drop Cast

3,8 · 2.5 Electrocatalytic measurements; 3.2

Metal precursors4-BNZ active material already synthesised
Linker precursorsin active material
Solventsslurry solvent not stated
Additives10 mg carbon black; 10 mg PVDF binder
Atmospherenot stated
Temperature80
Time24
Substrate orientationNickel foam, electrode area 1 x 1 cm
Oxidant / reductantnone during electrode fabrication
Work-upSlurry drop-cast onto nickel foam substrate
Activationdried for 1 day at 80 deg C; electrochemical activation by 100 CV cycles at 100 mV/s before tests
Scalability contextElectrode ink uses 80 wt% active material, 10 wt% carbon black, 10 wt% PVDF by stated masses; slurry solvent not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Other4-BNZ80 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Additivecarbon black10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
AdditivePVDF (polyvinylidene difluoride)10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Othernickel foam1 x 1 cm working area; 1.5 mm thickness3,8 · 2.5 Electrocatalytic measurements; 3.2
Complete recipeSource: Both

Route 7: Other

2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1

Metal precursors0.05 g pre-synthesised Ni-ZIF
Linker precursorsNi-ZIF framework contains 2-methylimidazolate linker
Solvents25 mL water for NaBH4 solution; DI water and ethanol washing
Additivesnone reported
Atmosphereroom temperature; atmosphere not stated
Temperatureroom temperature for boronization; 80 deg C drying
Time9
Substrate orientationnone; powder immersion
Oxidant / reductantNaBH4 (sodium borohydride), 1 M, reductant and boron source
Work-upResidue taken out and cleaned with DI water and ethanol six times
Activationovernight dried at 80 deg C
Scalability contextBatch powder immersion; no yield or scale-up reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi-ZIF0.05 g2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
ReductantNaBH4 (sodium borohydride)25 ml water + 1 M sodium borohydride solution · 1 M2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventwater25 ml2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
SolventDI waterwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Solventethanolwash 6 times2 · 2.3 Preparation of boronized Ni-ZIF (BNZ) · Fig. 1
Partial recipeSource: Both

Route 8: Drop Cast

3,8 · 2.5 Electrocatalytic measurements; 3.2

Metal precursors9-BNZ active material already synthesised
Linker precursorsin active material
Solventsslurry solvent not stated
Additives10 mg carbon black; 10 mg PVDF binder
Atmospherenot stated
Temperature80
Time24
Substrate orientationNickel foam, electrode area 1 x 1 cm
Oxidant / reductantnone during electrode fabrication
Work-upSlurry drop-cast onto nickel foam substrate
Activationdried for 1 day at 80 deg C; electrochemical activation by 100 CV cycles at 100 mV/s before tests
Scalability contextElectrode ink uses 80 wt% active material, 10 wt% carbon black, 10 wt% PVDF by stated masses; slurry solvent not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Other9-BNZ80 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Additivecarbon black10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
AdditivePVDF (polyvinylidene difluoride)10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Othernickel foam1 x 1 cm working area; 1.5 mm thickness3,8 · 2.5 Electrocatalytic measurements; 3.2
Partial recipeSource: Both

Route 9: Drop Cast

3,8 · 2.5 Electrocatalytic measurements; 3.2

Metal precursorsNZ active material already synthesised
Linker precursorsin active material
Solventsslurry solvent not stated
Additives10 mg carbon black; 10 mg PVDF binder
Atmospherenot stated
Temperature80
Time24
Substrate orientationNickel foam, electrode area 1 x 1 cm
Oxidant / reductantnone during electrode fabrication
Work-upSlurry drop-cast onto nickel foam substrate
Activationdried for 1 day at 80 deg C; electrochemical activation by 100 CV cycles at 100 mV/s before tests
Scalability contextElectrode ink uses 80 wt% active material, 10 wt% carbon black, 10 wt% PVDF by stated masses; slurry solvent not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherNZ80 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Additivecarbon black10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
AdditivePVDF (polyvinylidene difluoride)10 mg3,8 · 2.5 Electrocatalytic measurements; 3.2
Othernickel foam1 x 1 cm working area; 1.5 mm thickness3,8 · 2.5 Electrocatalytic measurements; 3.2
Complete recipeSource: Both

Route 10: Solvothermal

2 · 2.2 Preparation of Ni-ZIF (NZ)

Metal precursors0.1 M Ni(NO3)2.6H2O in 40 mL methanol
Linker precursors0.7 M 2-methylimidazole in 40 mL methanol
Solventsmethanol; DI water and ethanol for washing
Additivesnone reported
Atmospherenot stated
Temperature180
Time6
Substrate orientationnone; powder synthesis in 100 mL stainless steel autoclave
Oxidant / reductantnone reported
Work-upResidue cleaned with DI water and ethanol six times
Activationovernight dried at 80 deg C
Scalability contextPowder route; no scale-up data reported.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel nitrate hexahydrate (Ni(NO3)2.6H2O)40 ml solution · 0.1 M2 · 2.2 Preparation of Ni-ZIF (NZ)
Linker2-Methylimidazole40 ml solution · 0.7 M2 · 2.2 Preparation of Ni-ZIF (NZ)
SolventMethanol40 ml + 40 ml2 · 2.2 Preparation of Ni-ZIF (NZ)
SolventDI waterwash 6 times2 · 2.2 Preparation of Ni-ZIF (NZ)
Solventethanolwash 6 times2 · 2.2 Preparation of Ni-ZIF (NZ)