Synthesis evidence

Self-supporting electrocatalyst constructed from in-situ transformation of Co(OH)2 to metal-organic framework to Co/CoP/NC nanosheets for high-current-density water splitting

Chen N., Che S., Yuan Y. et al. · Journal of Colloid and Interface Science · 2023 · 513-524

8 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

p003 / journal page 515 · 2.4 Synthesis of Co/CoP/NC/CoF · Figure S3

Metal precursorsCo-MOF/CoF
Linker precursors2-MeIM-derived Co-MOF
AdditivesNaH2PO2
AtmosphereAr flow, 100 mL min^-1
Temperature350, 450, 550, or 650; optimized 550
Time2
Substrate orientationCo-MOF/CoF sample in tube furnace
Oxidant / reductantNaH2PO2 phosphorus source; PH3 generated by decomposition noted in text
Activationramp rate 5 C min^-1
Scalability contextSelf-supporting electrode used directly without binder or conductive additive.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo-MOF/CoFNot specifiedp003 / journal page 515 · 2.4 Synthesis of Co/CoP/NC/CoF · Figure S3
Reductantsodium hypophosphite (NaH2PO2)Not specifiedp003 / journal page 515 · 2.4 Synthesis of Co/CoP/NC/CoF · Figure S3
OtherAr100 mL min^-1p003 / journal page 515 · 2.4 Synthesis of Co/CoP/NC/CoF · Figure S3
Partial recipeSource: Both

Route 2: Other

p003 / journal page 515 · 2.3 Synthesis of Co-MOF/CoF · Figure S1-S2

Metal precursorsCo2+ exposed/released from Co(OH)2/CoF; no exogenous metal ions
Linker precursors2-methylimidazole
Solventsaqueous 2-MeIM solution
Atmosphereambient
Temperatureroom temperature not explicitly stated for endogenous route
Time1, 3, 6, or 12; optimized 6
Oxidant / reductantdynamic dissolution-coordination of Co(OH)2 to Co2+
Work-upwashed with ethanol and dried
Scalability contextNo exogenous metal source; organic ligands can be recycled repeatedly according to conclusion.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(OH)2/CoFNot specifiedp003 / journal page 515 · 2.3 Synthesis of Co-MOF/CoF · Figure S1-S2
Linker2-methylimidazole (2-MeIM)2 mol L^-1p003 / journal page 515 · 2.3 Synthesis of Co-MOF/CoF · Figure S1-S2
SolventwaterNot specifiedp003 / journal page 515 · 2.3 Synthesis of Co-MOF/CoF · Figure S1-S2
Solventethanolwashp003 / journal page 515 · 2.3 Synthesis of Co-MOF/CoF · Figure S1-S2
Complete recipeSource: Main

Route 3: Other

p003 / journal page 515 · 2.2 In-situ etching growth

Metal precursorscobalt foam
Solventsethyl alcohol; acetone; hydrochloric acid; ethanol rinse
Atmosphereambient
Temperatureroom temperature
Time0.333 h in each cleaning solvent
Work-upwashed with ethanol several times
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoF2 cm x 4 cmp003 / journal page 515 · 2.2 In-situ etching growth
Solventethyl alcoholNot specifiedp003 / journal page 515 · 2.2 In-situ etching growth
SolventacetoneNot specifiedp003 / journal page 515 · 2.2 In-situ etching growth
Acidhydrochloric acidNot specifiedp003 / journal page 515 · 2.2 In-situ etching growth
SolventethanolNot specifiedp003 / journal page 515 · 2.2 In-situ etching growth
Complete recipeSource: Both

Route 4: Hydrothermal

p003 / journal page 515 · 2.2 In-situ etching growth · Formula S1-S3 in SI

Metal precursorscobalt foam
Solventsdeionized water
Atmosphereambient
Temperature80
Time3
Oxidant / reductantwater and dissolved oxygen participate in corrosion/etching according to SI formulas S1-S3
Work-uprepeatedly cleaned with ethanol and air-dried at room temperature
Scalability contextAuthors describe the strategy as simple, universal, low-cost and suitable for large-scale industrialisation.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoFcleaned 2 cm x 4 cm piecep003 / journal page 515 · 2.2 In-situ etching growth · Formula S1-S3 in SI
Solventdeionized waterNot specifiedp003 / journal page 515 · 2.2 In-situ etching growth · Formula S1-S3 in SI
Solventethanolwashp003 / journal page 515 · 2.2 In-situ etching growth · Formula S1-S3 in SI
Complete recipeSource: Main

Route 5: Other

p003 / journal page 515 · 2.6 Synthesis of CoP/CoF nanosheets

Metal precursorsCo(OH)2/CoF
AdditivesNaH2PO2
AtmosphereAr flow, 100 mL min^-1
Temperature550
Time2
Substrate orientationNaH2PO2 in upstream boat, Co(OH)2/CoF in downstream boat in tube furnace
Oxidant / reductantNaH2PO2 phosphorus source
Activationramp rate 5 C min^-1
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(OH)2/CoFNot specifiedp003 / journal page 515 · 2.6 Synthesis of CoP/CoF nanosheets
ReductantNaH2PO21 gp003 / journal page 515 · 2.6 Synthesis of CoP/CoF nanosheets
OtherAr100 mL min^-1p003 / journal page 515 · 2.6 Synthesis of CoP/CoF nanosheets
Partial recipeSource: Main

Route 6: Other

p003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF

Metal precursorsExo-Co-MOF/CoF
Linker precursors2-MeIM-derived exogenous Co-MOF
AdditivesNaH2PO2
AtmosphereAr flow, 100 mL min^-1
Temperature550
Time2
Oxidant / reductantNaH2PO2 phosphorus source
Activationramp rate 5 C min^-1
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceExo-Co-MOF/CoFNot specifiedp003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
Reductantsodium hypophosphite (NaH2PO2)Not specifiedp003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
OtherAr100 mL min^-1p003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
Partial recipeSource: Main

Route 7: Other

p003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF

Metal precursorsCoF and Co(NO3)2
Linker precursors2-methylimidazole
Solventsaqueous solution
Atmosphereambient
Temperatureroom temperature
Time6
Work-upwashed with ethanol and dried
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCoFNot specifiedp003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
Metal Sourcecobalt nitrate hexahydrate (Co(NO3)2 6H2O)0.5 mol L^-1p003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
Linker2-methylimidazole (2-MeIM)2 mol L^-1p003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
SolventwaterNot specifiedp003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
Solventethanolwashp003 / journal page 515 · 2.5 Synthesis of Exo-Co/CoP/NC/CoF
Complete recipeSource: Main

Route 8: Drop Cast

p003 / journal page 515 · 2.8 Electrochemical measurements

Metal precursorscommercial Pt/C or RuO2 powder
Solventsethanol and deionized water
AdditivesNafion (5%)
Atmosphereambient
Temperatureroom temperature
Time0.5 h ultrasonication
Substrate orientationdrop-cast ink on electrode
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherPt/C (20 wt%) or RuO25.0 mgp003 / journal page 515 · 2.8 Electrochemical measurements
Solventethanol250 uLp003 / journal page 515 · 2.8 Electrochemical measurements
Solventdeionized water250 uLp003 / journal page 515 · 2.8 Electrochemical measurements
AdditiveNafion20 uL · 5%p003 / journal page 515 · 2.8 Electrochemical measurements