Synthesis evidence

Toward Enhancing Performance of Electromagnetic Wave Absorption for Conductive Metal-Organic Frameworks: Nanostructure Engineering or Crystal Morphology Controlling

Wang X., Zhang X., He A. et al. · Inorganic Chemistry · 2024 · 6948-6956

3 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

2 · 2.1. Synthesis of A-Cu-HHTP

Metal precursorsCu(NO3)2.3H2O (0.263 mmol, 0.063 g)
Linker precursorsHHTP (0.159 mmol, 0.051 g)
Solventsdeionized water: 1.0 mL for solution A and 4.1 mL for solution B
Additives25 wt% aqueous ammonia solution (7.95 mmol, 1.2 mL); final mixed-solution pH approximately 10
Atmospherenot reported
Temperature85
Time24
Work-upcool to room temperature; collect black precipitate by centrifugation; wash with H2O and EtOH; dry in vacuum oven at 60 C
ActivationBET degassing separately reported at 120 C for 8 h before porosity measurement
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2O0.263 mmol, 0.063 g2 · 2.1. Synthesis of A-Cu-HHTP
Base25 wt % aqueous ammonia solution7.95 mmol, 1.2 mL · 25 wt %2 · 2.1. Synthesis of A-Cu-HHTP
LinkerHHTP0.159 mmol, 0.051 g2 · 2.1. Synthesis of A-Cu-HHTP
Solventdeionized water1.0 mL + 4.1 mL2 · 2.1. Synthesis of A-Cu-HHTP
SolventEtOHwash solvent · 99% in SI materials list2 · 2.1. Synthesis of A-Cu-HHTP
Complete recipeSource: Both

Route 2: Hydrothermal

2 · 2.2. Synthesis of B-Cu-HHTP

Metal precursorsCu(OAc)2.H2O (0.080 mmol, 0.020 g)
Linker precursorsHHTP (0.043 mmol, 0.014 g)
Solvents8 mL deionized water
Additivesnone reported; final mixed-solution pH approximately 3
Atmospherenot reported
Temperature85
Time12
Work-upultrasound 15 min; transfer to 23 mL Teflon autoclave; cool to room temperature; collect black precipitate by centrifugation; wash with H2O and EtOH; dry in vacuum oven at 60 C overnight
ActivationBET degassing separately reported at 120 C for 8 h before porosity measurement
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHHTP0.043 mmol, 0.014 g2 · 2.2. Synthesis of B-Cu-HHTP
Metal SourceCu(OAc)2.H2O0.080 mmol, 0.020 g2 · 2.2. Synthesis of B-Cu-HHTP
Solventdeionized water8 mL2 · 2.2. Synthesis of B-Cu-HHTP
SolventEtOHwash solvent · 99% in SI materials list2 · 2.2. Synthesis of B-Cu-HHTP
Partial recipeSource: Both

Route 3: Hydrothermal

2 · 2.3. Synthesis of C-Cu-HHTP

Metal precursorsCu(NO3)2.3H2O inferred same as A-Cu-HHTP recipe
Linker precursorsHHTP inferred same as A-Cu-HHTP recipe
Solventsdeionized water inferred same as A-Cu-HHTP recipe
Additivespyridine replaces 25 wt% aqueous ammonia solution; final mixed-solution pH approximately 5
Atmospherenot reported
Temperature85
Time24
Work-upreported as similar to A-Cu-HHTP; inferred cool, centrifuge, wash with H2O and EtOH, dry in vacuum oven at 60 C
ActivationBET degassing separately reported at 120 C for 8 h before porosity measurement
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)2.3H2Oinferred same as A-Cu-HHTP; exact amount not repeated2 · 2.3. Synthesis of C-Cu-HHTP
LinkerHHTPinferred same as A-Cu-HHTP; exact amount not repeated2 · 2.3. Synthesis of C-Cu-HHTP
Basepyridinenot reported · 99% in SI materials list2 · 2.3. Synthesis of C-Cu-HHTP
Solventdeionized waterinferred same as A-Cu-HHTP2 · 2.3. Synthesis of C-Cu-HHTP