Synthesis evidence

Boosting the Optoelectronic Performance by Regulating Exciton Behaviors in a Porous Semiconductive Metal-Organic Framework

Liang C., Cheng L., Zhang S. et al. · Journal of the American Chemical Society · 2022 · 2189-2196

6 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

p003 / SI S1 · Synthesis of the mechanical mixture

Metal precursorsTbTATAB component
Linker precursorsTATAB3- framework in TbTATAB
AdditivesRhB
Atmosphereambient/not specified
Work-upmixed well in a mortar
Activationpressed to a wafer for detector reference
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTbTATAB100 mgp003 / SI S1 · Synthesis of the mechanical mixture
AdditiveRhB1.64 mgp003 / SI S1 · Synthesis of the mechanical mixture
Complete recipeSource: SI

Route 2: Other

p003 / SI S1 · Synthesis of the mechanical mixture; X-ray detection experiment · Figure S25

Metal precursorsmechanical mixture containing TbTATAB
Linker precursorsTATAB3- framework in mixture
AdditivesRhB; Ag electrodes
Atmosphereambient/not specified
Substrate orientationAg/sample/Ag sandwich
Work-upmixed in mortar and pressed to wafer; device processed as Ag/sample/Ag
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othermechanical mixture15 mg wafer used for detector protocolp003 / SI S1 · Synthesis of the mechanical mixture; X-ray detection experiment · Figure S25
OtherAg electrodesAg/sample/Agp003 / SI S1 · Synthesis of the mechanical mixture; X-ray detection experiment · Figure S25
Complete recipeSource: Both

Route 3: Other

p003 / SI S1 · Synthesis of RhB+@TbTATAB · Figures S1, S9-S14

Metal precursorspreformed TbTATAB (200 mg)
Linker precursorspreformed TbTATAB framework
Solvents80 mL rhodamine B solution; solvent not explicitly specified in synthesis paragraph
Additivesrhodamine B (RhB), 0.1 mmol/L
Atmosphereambient/not specified; shaker
Temperatureroom temperature/not specified
Time2
Work-upcentrifugation; washed three times with EtOH to remove surface RhB
Activationdried in vacuum for 1 h at 60 degC
Scalability contextAdsorbed content 16.42 mg/g, corresponding in the main text to 66.5 mmol RhB+/mol TbTATAB.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherTbTATAB200 mgp003 / SI S1 · Synthesis of RhB+@TbTATAB · Figures S1, S9-S14
Additiverhodamine B (RhB) solution80 mL · 0.1 mmol/Lp003 / SI S1 · Synthesis of RhB+@TbTATAB · Figures S1, S9-S14
SolventEtOH washwashed three timesp003 / SI S1 · Synthesis of RhB+@TbTATAB · Figures S1, S9-S14
Complete recipeSource: SI

Route 4: Other

p003 / SI S1 · Fabrication of pelleted wafer-based detectors · Figure S22

Metal precursorsRhB+@TbTATAB powder/crystals
Linker precursorsRhB+@TbTATAB powder/crystals
AdditivesAg electrodes
Atmosphereambient/not specified
Substrate orientationcathode irradiation configuration; Ag/sample/Ag sandwich
Work-uppreground in mortar; pelleted at 15 MPa in 3 mm mold; 15 mg wafer
Scalability contextWafer thickness considered separately, approximately 1.3 mm.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherRhB+@TbTATAB sample15 mg waferp003 / SI S1 · Fabrication of pelleted wafer-based detectors · Figure S22
OtherAg electrodesAg/sample/Agp003 / SI S1 · Fabrication of pelleted wafer-based detectors · Figure S22
Complete recipeSource: SI

Route 5: Other

p003 / SI S1 · X-ray detection experiment · Figure S24

Metal precursorsTbTATAB powder/crystals
Linker precursorsTbTATAB powder/crystals
AdditivesAg electrodes
Atmosphereambient/not specified
Substrate orientationcathode irradiation configuration; Ag/sample/Ag sandwich
Work-uppreground in mortar; pelleted at 15 MPa in 3 mm mold; 15 mg wafer
Scalability contextWafer thickness considered separately, approximately 1.3 mm.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherTbTATAB sample15 mg waferp003 / SI S1 · X-ray detection experiment · Figure S24
OtherAg electrodesAg/sample/Agp003 / SI S1 · X-ray detection experiment · Figure S24
Complete recipeSource: Both

Route 6: Solvothermal

p003 / SI S1 · Synthesis of TbTATAB

Metal precursorsTb(NO3)3.6H2O (0.1 mmol, 0.0435 g)
Linker precursorsH3TATAB (0.05 mmol, 0.025 g)
Solventsdeionized water (2 mL) and DMF (6 mL)
Atmospheresealed 10 mL glass vial; atmosphere not otherwise specified
Temperature100
Time72
Work-upcooled to room temperature; rinsed with DMF 3 times; rinsed with ethanol
Activationdried in vacuum for 1 h at 60 degC
Scalability contextProduct yield 79% based on Tb.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceTb(NO3)3.6H2O0.1 mmol, 0.0435 gp003 / SI S1 · Synthesis of TbTATAB
LinkerH3TATAB0.05 mmol, 0.025 gp003 / SI S1 · Synthesis of TbTATAB
Solventdeionized water2 mLp003 / SI S1 · Synthesis of TbTATAB
SolventDMF6 mLp003 / SI S1 · Synthesis of TbTATAB