Synthesis evidence

Oriented Growth of In-Oxo Chain Based Metal-Porphyrin Framework Thin Film for High-Sensitive Photodetector

Tian Y.-B., Vankova N., Weidler P. et al. · Advanced Science · 2021 · 2100548

4 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

5 · Fabrication of In-TCPP SURMOF and mix-oriented thin film

Metal precursorsindium nitrate / In(NO3)3
Linker precursorsTCPP, 5,10,15,20-tetra(4-carboxyphenyl)porphyrin
Solventsethanol for diluted precursor solutions and rinsing
AdditivesNaOH and 30% H2O2 used for substrate OH-functionalisation
Atmospheredried under nitrogen flux after substrate functionalisation; growth atmosphere not reported
Temperature80 for substrate functionalisation; room temperature not explicitly reported for LPE dipping
Time0.333 h In(NO3)3 immersion and 0.5 h TCPP immersion per cycle; 0.5 h substrate functionalisation
Substrate orientationOH-functionalised SiO2/Si; [021] orientation perpendicular to the substrate in the resulting SURMOF
Oxidant / reductant30% hydrogen peroxide in substrate pretreatment
Work-upEach precursor immersion step followed by rinsing with pure ethanol to remove residual reactants.
Activationnot reported
Scalability contextLayer-by-layer cycles tune thickness from approximately 60 to 240 nm for 5-20 cycles.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceindium nitrate1 mM5 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
LinkerTCPP0.1 mM5 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
SolventethanolNot specified5 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
BaseNaOH solutionmixture with 30% hydrogen peroxide, ratio 3:1 · 2 mM5 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
Oxidanthydrogen peroxidemixture with 2 mM NaOH, ratio 3:1 · 30%5 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
Complete recipeSource: SI

Route 2: Solvothermal

5-6 · Fabrication of In-TCPP SURMOF and mix-oriented thin film

Metal precursorsIndium nitrate (150 mg, 0.5 mmol)
Linker precursors5,10,15,20-tetra(4-carboxyphenyl)porphyrin (TCPP) (158 mg, 0.2 mmol)
SolventsDMF (10 mL); DMF and ethanol wash
Atmospheresealed glass bottle; vacuum drying after wash
Temperature120
Time24
Substrate orientationfunctional substrate in solution; final mixed-orientation film assembled on SiO2/Si substrate
Work-upWashed with DMF and ethanol in turn.
Activationdried in vacuum at 60 deg C
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceIndium nitrate150 mg, 0.5 mmol5-6 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
Linker5,10,15,20-tetra(4-carboxyphenyl) porphyrin (TCPP)158 mg, 0.2 mmol5-6 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
SolventDMF10 ml5-6 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
Solventethanolwash5-6 · Fabrication of In-TCPP SURMOF and mix-oriented thin film
Partial recipeSource: SI

Route 3: Other

6 · Fabrication of In-TCPP based photodetector · Figure 3a

Metal precursorssilver electrode vapour
Additivescopper interdigital electrode grid as shadow mask
Atmospherethermal evaporation chamber
Substrate orientationAg electrodes patterned on the surface of the MOF thin film
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OthersilverAg vapors6 · Fabrication of In-TCPP based photodetector · Figure 3a
Othercopper interdigital electrode gridsshadow mask6 · Fabrication of In-TCPP based photodetector · Figure 3a
Partial recipeSource: SI

Route 4: Other

6 · in-situ monitoring the growth process of In-TCPP SURMOF · Figure S2

Metal precursorsIn(NO3)3 solution
Linker precursorsTCPP solution
Solventsethanol baseline and rinse
Additives11-mercapto-1-undecanol SAM on Au chip
Atmosphereliquid phase flow module; atmosphere not reported
Temperature50
Substrate orientationMUD SAM-functionalised Au-coated QCM working electrode
Work-upPure ethanol used for baseline and rinsing between precursor flows.
Activationnot reported
Scalability contextQCM-D monitoring experiment rather than preparative device route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceIn(NO3)31 mM6 · in-situ monitoring the growth process of In-TCPP SURMOF · Figure S2
LinkerTCPP0.2 mM, equimolar6 · in-situ monitoring the growth process of In-TCPP SURMOF · Figure S2
Solventethanolbaseline and rinsing step6 · in-situ monitoring the growth process of In-TCPP SURMOF · Figure S2
Additive11-mercapto-1-undecanol (MUD) SAMNot specified6 · in-situ monitoring the growth process of In-TCPP SURMOF · Figure S2