Synthesis evidence

Facile interfacial charge transfer across hole doped cobalt-based MOFs/TiO2 nano-hybrids making MOFs light harvesting active layers in solar cells

Lee D.Y., Lim I., Shin C.Y. et al. · Journal of Materials Chemistry A · 2015 · 22669-22676

7 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

p002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs

Metal precursorsCo(NO3)2.3H2O, 0.137 mM
Linker precursorsterephthalic acid, 0.137 mM
SolventsDMF/ethanol, 1:4 volume ratio
Atmospherenot reported
Temperature100
Time15
Work-upFiltered, washed thoroughly with DMF, dried at 50 C for 3 h.
Activationnot reported
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2.3H2O0.137 mMp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
Linkerterephthalic acid0.137 mMp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
SolventDMF1:4 volume ratio of DMF and ethanolp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
Solventethanol1:4 volume ratio of DMF and ethanolp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
Partial recipeSource: Main

Route 2: Other

p002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode

Metal precursorsCo(NO3)2.3H2O in DMF, 0.1 M
Linker precursorsbenzenedicarboxylic acid in DMF, 0.1 M
SolventsDMF
Atmospherenot reported
Temperature120
Time40 h total dipping time for 20 cycles (1 h linker + 1 h metal per cycle)
Substrate orientationTiO2 modified FTO
Work-upDMF wash after each linker and metal dipping step.
Activationnot reported
Scalability context20 LBL cycles were selected after hit-and-trial J-V optimisation.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linkerbenzenedicarboxylic acid0.1 Mp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
Metal SourceCo(NO3)2.3H2O0.1 Mp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
SolventDMFNot specifiedp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
Partial recipeSource: Main

Route 3: Other

p002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode

Solventsacetonitrile
Atmospherenot reported
Temperature50
Time2
Substrate orientationapplies to Co-BDC and Co-NDC films on glass and TiO2/FTO
Oxidant / reductantI2 oxidant, 0.1 M
Work-upWashed thoroughly with acetonitrile to remove physically adsorbed iodine.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OxidantI20.1 Mp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
SolventacetonitrileNot specifiedp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
Partial recipeSource: Main

Route 4: Solvothermal

p002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs

Metal precursorsCo(NO3)2.3H2O, 0.344 mM
Linker precursors2,6-NDC (2,6-naphthalenedicarboxylic acid), 0.115 mM
SolventsDMF
Atmospherenot reported
Temperature180
Time72
Work-upFiltered, washed thoroughly with DMF, dried at 50 C for 3 h.
Activationnot reported
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(NO3)2.3H2O0.344 mMp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
Linker2,6-NDC (2,6-naphthalenedicarboxylic acid)0.115 mMp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
SolventDMFNot specifiedp002 / article p.22670 · Experimental - Synthesis of bulk Co-MOFs
Partial recipeSource: Main

Route 5: Other

p002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode

Metal precursorsCo(NO3)2.3H2O in DMF, 0.1 M
Linker precursors2,6-naphthalenedicarboxylic acid in DMF, 0.1 M
SolventsDMF
Atmospherenot reported
Temperature120
Time40 h total dipping time for 20 cycles (1 h linker + 1 h metal per cycle)
Substrate orientationTiO2 modified FTO
Work-upDMF wash after each linker and metal dipping step.
Activationnot reported
Scalability context20 LBL cycles were selected after hit-and-trial J-V optimisation.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,6-naphthalenedicarboxylic acid0.1 Mp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
Metal SourceCo(NO3)2.3H2O0.1 Mp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
SolventDMFNot specifiedp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode
Partial recipeSource: Main

Route 6: Other

p002 / article p.22670 · Experimental - Preparation of the hole blocking layer

Metal precursorstitanium-diisopropoxide bis(acetylacetonate), 0.15 M
Solvents1-butanol
Atmosphereair implied; not explicitly reported
Temperature500
Time0.333
Substrate orientationcleaned FTO glass
Work-upSpin-coated at 2000 rpm for 30 s, annealed at 500 C for 20 min.
Activationannealing at 500 C
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othertitanium-diisopropoxide bis(acetylacetonate)a few drops · 0.15 Mp002 / article p.22670 · Experimental - Preparation of the hole blocking layer
Solvent1-butanolNot specifiedp002 / article p.22670 · Experimental - Preparation of the hole blocking layer
Partial recipeSource: Main

Route 7: Other

p002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode

Metal precursorscommercial TiO2 nanoparticle paste (TTP-20N, ENB Korea)
Atmosphereair implied; not explicitly reported
Temperature450
Time0.5
Substrate orientationHBL-coated FTO glass
Work-upDoctor-bladed onto HBL-coated FTO and sintered at 450 C for 30 min.
Activationsintering at 450 C
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherTiO2 nanoparticle paste (TTP-20N, ENB Korea)Not specifiedp002 / article p.22670 · Experimental - Preparation, sensitization and doping of the TiO2 photoanode