Synthesis evidence

Metal-organic frameworks with fine-tuned interlayer spacing for microwave absorption

Zhang X., Tian X., Wu N. et al. · Science Advances · 2024 · eadl6498

7 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Hydrothermal

7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP

Metal precursors0.5 mmol anhydrous copper acetate [Cu(CH3COO)2]
Linker precursors0.3 mmol HHTP
Solvents10 mL H2O for metal salt solution; 10 mL isopropanol for HHTP dispersion
Atmospherenot specified
Temperature85
Time15
Work-upProducts obtained by centrifugation, washed with water and ethanol.
ActivationDried at 50 C for 12 h.
Scalability contextAuthors state quick addition gives higher reaction rates and production yields but lower crystallinity.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous copper acetate [Cu(CH3COO)2]0.5 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
LinkerHHTP0.3 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
SolventH2O10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Solventisopropanol10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Complete recipeSource: Main

Route 2: Hydrothermal

7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP

Metal precursors0.125 mmol Zn(CH3COO)2 and 0.375 mmol Cu(CH3COO)2
Linker precursors0.3 mmol HHTP
Solvents10 mL H2O; 10 mL isopropanol
Atmospherenot specified
Temperature85
Time15
Work-upCentrifugation, washing with water and ethanol.
ActivationDried at 50 C for 12 h.
Scalability contextQuick metal-solution addition was used for efficient comparison.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous zinc acetate [Zn(CH3COO)2]0.125 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Metal Sourceanhydrous copper acetate [Cu(CH3COO)2]0.375 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
LinkerHHTP0.3 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
SolventH2O10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Solventisopropanol10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Complete recipeSource: Main

Route 3: Hydrothermal

7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP

Metal precursors0.25 mmol Zn(CH3COO)2 and 0.25 mmol Cu(CH3COO)2
Linker precursors0.3 mmol HHTP
Solvents10 mL H2O; 10 mL isopropanol
Atmospherenot specified
Temperature85
Time15
Work-upCentrifugation, washing with water and ethanol.
ActivationDried at 50 C for 12 h.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous zinc acetate [Zn(CH3COO)2]0.25 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Metal Sourceanhydrous copper acetate [Cu(CH3COO)2]0.25 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
LinkerHHTP0.3 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
SolventH2O10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Solventisopropanol10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Complete recipeSource: Main

Route 4: Hydrothermal

7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP

Metal precursors0.375 mmol Zn(CH3COO)2 and 0.125 mmol Cu(CH3COO)2
Linker precursors0.3 mmol HHTP
Solvents10 mL H2O; 10 mL isopropanol
Atmospherenot specified
Temperature85
Time15
Work-upCentrifugation, washing with water and ethanol.
ActivationDried at 50 C for 12 h.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous zinc acetate [Zn(CH3COO)2]0.375 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Metal Sourceanhydrous copper acetate [Cu(CH3COO)2]0.125 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
LinkerHHTP0.3 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
SolventH2O10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Solventisopropanol10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Complete recipeSource: Main

Route 5: Hydrothermal

7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP

Metal precursors0.5 mmol Zn(CH3COO)2
Linker precursors0.3 mmol HHTP
Solvents10 mL H2O; 10 mL isopropanol
Atmospherenot specified
Temperature85
Time15
Work-upCentrifugation, washing with water and ethanol.
ActivationDried at 50 C for 12 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous zinc acetate [Zn(CH3COO)2]0.5 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
LinkerHHTP0.3 mmol7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
SolventH2O10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Solventisopropanol10 ml7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Partial recipeSource: Main

Route 6: Hydrothermal

7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP

Metal precursorsZn(CH3COO)2/Cu(CH3COO)2 aqueous solutions at the ZnCu-HHTP ratios
Linker precursors0.3 mmol HHTP dispersed in isopropanol
SolventsH2O and isopropanol
Atmospherenot specified
Temperature85
Time15
Work-upNot separately specified; inferred to follow centrifugation, washing and drying from the standard route.
ActivationDried at 50 C for 12 h in the standard route; not separately specified for the slow-addition variant.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous zinc acetate [Zn(CH3COO)2]varied by Zn/Cu ratio7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Metal Sourceanhydrous copper acetate [Cu(CH3COO)2]varied by Zn/Cu ratio7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
LinkerHHTP0.3 mmol in standard route7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
SolventH2O/isopropanol10 ml/10 ml in standard route7 · Synthesis of ZnCu-HHTP, Zn-HHTP, and Cu-HHTP
Partial recipeSource: Main

Route 7: Hydrothermal

7 · Synthesis of ZnNi-HHTP, Ni-HHTP

Metal precursorsZn(CH3COO)2 and Ni(CH3COO)2.4H2O replacing Cu(CH3COO)2 in the ZnCu-HHTP route
Linker precursorsHHTP
SolventsH2O and isopropanol
Atmospherenot specified
Temperature85
Time15
Work-upInferred same centrifugation, water/ethanol washing, and 50 C drying as ZnCu-HHTP.
ActivationDried at 50 C for 12 h by same method; exact wording not repeated for ZnNi route.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourceanhydrous zinc acetate [Zn(CH3COO)2]varied by Zn/Ni ratio7 · Synthesis of ZnNi-HHTP, Ni-HHTP
Metal Sourcenickel acetate [Ni(CH3COO)2.4H2O]varied by Zn/Ni ratio7 · Synthesis of ZnNi-HHTP, Ni-HHTP
LinkerHHTPsame as ZnCu-HHTP route7 · Synthesis of ZnNi-HHTP, Ni-HHTP
SolventH2O/isopropanolsame as ZnCu-HHTP route7 · Synthesis of ZnNi-HHTP, Ni-HHTP