Synthesis evidence

Embedding Pt in Ni-MOF/CdS organic-inorganic hybrid materials as electron channel to promote photogenerated carrier separation for enhanced photocatalytic hydrogen evolution under visible light

Lu Y., Wang Y., Liu J. et al. · Separation and Purification Technology · 2024 · 128000

10 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

2 · 2.3

Metal precursorsNiCl2.6H2O varied; 0.2 mmol inferred from sample name
Linker precursorsterephthalic acid varied; 0.2 mmol inferred from sample name
SolventsDMF / anhydrous ethanol / DI water as for 0.3 NPC
Atmospherenot specified
Temperature140
Time24
Work-upWash with anhydrous ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acid0.2 mmol inferred from sample name2 · 2.3
Metal SourceNiCl2.6H2O0.2 mmol inferred from sample name2 · 2.3
OtherPCnot restated2 · 2.3
Complete recipeSource: Main

Route 2: Solvothermal

2 · 2.3 · Fig. 1c

Metal precursorsNiCl2.6H2O, 0.3 mmol; PC, 1 mmol
Linker precursorsterephthalic acid, 0.3 mmol
SolventsDMF 32 mL; anhydrous ethanol 2 mL; DI water 2 mL
Atmospherenot specified
Temperature140
Time24
Work-upWash with anhydrous ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Scalability context50 mL Teflon-lined autoclave batch.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
SolventDMF (68-12-2)32 ml2 · 2.3 · Fig. 1c
Solventanhydrous ethanol2 ml2 · 2.3 · Fig. 1c
SolventDI water2 ml2 · 2.3 · Fig. 1c
Linkerterephthalic acid (100-21-0)0.3 mmol2 · 2.3 · Fig. 1c
Metal SourceNiCl2.6H2O (7791-20-0)0.3 mmol2 · 2.3 · Fig. 1c
OtherPC1 mmol2 · 2.3 · Fig. 1c
Partial recipeSource: Main

Route 3: Solvothermal

2 · 2.3

Metal precursorsNiCl2.6H2O varied; 0.4 mmol inferred from sample name
Linker precursorsterephthalic acid varied; 0.4 mmol inferred from sample name
SolventsDMF / anhydrous ethanol / DI water as for 0.3 NPC
Atmospherenot specified
Temperature140
Time24
Work-upWash with anhydrous ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acid0.4 mmol inferred from sample name2 · 2.3
Metal SourceNiCl2.6H2O0.4 mmol inferred from sample name2 · 2.3
OtherPCnot restated2 · 2.3
Partial recipeSource: Main

Route 4: Solvothermal

2 · 2.3

Metal precursorsNiCl2.6H2O varied; 0.5 mmol inferred from sample name
Linker precursorsterephthalic acid varied; 0.5 mmol inferred from sample name
SolventsDMF / anhydrous ethanol / DI water as for 0.3 NPC
Atmospherenot specified
Temperature140
Time24
Work-upWash with anhydrous ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acid0.5 mmol inferred from sample name2 · 2.3
Metal SourceNiCl2.6H2O0.5 mmol inferred from sample name2 · 2.3
OtherPCnot restated2 · 2.3
Complete recipeSource: Main

Route 5: Hydrothermal

2 · 2.1 · Fig. 1a

Metal precursorsCd(NO3)2.4H2O, 10 mmol
Solventsethylenediamine, 25 mL
AdditivesCH4N2S / thiourea, 45 mmol
Atmospherenot specified
Temperature150
Time24
Work-upCool to ambient temperature; wash several times with DI water and ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Scalability context50 mL Teflon-lined autoclave batch.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCd(NO3)2.4H2O (CAS 10022-68-1)10 mmol2 · 2.1 · Fig. 1a
AdditiveCH4N2S (CAS 62-56-6)45 mmol2 · 2.1 · Fig. 1a
Solventethylenediamine25 ml2 · 2.1 · Fig. 1a
Partial recipeSource: Main

Route 6: Solvothermal

2 · 2.3

Metal precursorsNiCl2.6H2O; CdS
Linker precursorsterephthalic acid
SolventsDMF / anhydrous ethanol / DI water
Atmospherenot specified
Temperature140
Time24
Work-upAs above NPC method; wash with anhydrous ethanol and vacuum dry.
Activationvacuum drying at 60 deg C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2Onot fully restated; 0.3 mmol inferred for 0.3 NC2 · 2.3
Linkerterephthalic acidnot fully restated; 0.3 mmol inferred for 0.3 NC2 · 2.3
OtherCdSnot stated2 · 2.3
Vague recipeSource: Main

Route 7: Unknown

3-4 · 3.1 · Fig. 2b; Fig. 3c

Metal precursorsnot reported in supplied main text
Linker precursorsnot reported in supplied main text
Partial recipeSource: Main

Route 8: Solvothermal

2 · 2.3

Metal precursorsNiCl2.6H2O varied; exact amounts for 0.1/0.2/0.4/0.5 NPC not stated
Linker precursorsterephthalic acid varied; exact amounts for 0.1/0.2/0.4/0.5 NPC not stated
SolventsDMF / anhydrous ethanol / DI water as for 0.3 NPC
Atmospherenot specified
Temperature140
Time24
Work-upWash with anhydrous ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerterephthalic acidvaried2 · 2.3
Metal SourceNiCl2.6H2Ovaried2 · 2.3
OtherPCnot restated2 · 2.3
Complete recipeSource: Main

Route 9: Other

2 · 2.2 · Fig. 1b

Metal precursorsH2PtCl6.6H2O, 26.6 uL of 10 g/L mixture; CdS, 0.0999 g
Solventsethylene glycol, 30 mL + 5 mL
Atmospherenitrogen vented for 30 min
Temperature50
Time2
Oxidant / reductantethylene glycol likely acts as solvent/reducing medium; not explicitly described
Work-upCentrifugation washing with anhydrous ethanol; vacuum dry 24 h at 60 deg C.
Activationvacuum drying at 60 deg C for 24 h
Scalability context250 mL three-necked flask batch.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherCdS0.0999 g2 · 2.2 · Fig. 1b
Metal SourceH2PtCl6.6H2O (CAS 18497-13-7)26.6 uL · 10 g/L mixture2 · 2.2 · Fig. 1b
Solventethylene glycol (107-21-1)30 ml + 5 ml2 · 2.2 · Fig. 1b
Partial recipeSource: Main

Route 10: Other

2 · 2.3

Metal precursorsH2PtCl6.6H2O and NC
Linker precursorsterephthalic acid already in NC
Solventsethylene glycol, as Pt loading route
Atmospherenitrogen, inferred from Pt loading method
Temperature50
Time2
Oxidant / reductantethylene glycol likely acts as solvent/reducing medium; not explicitly described
Work-upAs Pt loading method: wash with anhydrous ethanol and vacuum dry.
Activationvacuum drying at 60 deg C for 24 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceH2PtCl6.6H2Onot restated for PNC · not restated; Pt loading method used 10 g/L mixture2 · 2.3
OtherNCnot stated2 · 2.3
Solventethylene glycolnot restated for PNC2 · 2.3