Synthesis evidence

Facile Preparation of Polymorphic Metal–Organic Framework Nanostructures as Microwave Absorbers via One-Pot Hydrothermal Reaction

Miao P., Zhang H., Zhang M. et al. · ACS Applied Nano Materials · 2026 · 1676-1687

4 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

1678-1679 · 2.2 / 3.1 · Figure 1

Metal precursorsCopper(I) iodide (AR, >=99%), 5 mmol
Linker precursorsTCNQ in acetonitrile; amount not reported in the methods passage
SolventsAcetonitrile, 100 mL TCNQ/acetonitrile solution
Atmosphereair/not specified
Temperature60 deg C in Figure 1/results discussion; methods passage only says stirred for 5 min
Time0.083 h by methods stirring time; discussion/Figure 1 imply 10 min
Oxidant / reductantCu(I) acts as in situ reductant for TCNQ
Work-upSeparated by filtration several times, washed with ethanol, dried at 65 deg C overnight.
ActivationNo activation reported beyond drying at 65 deg C overnight.
Scalability contextAuthors state high yield/no pyrolysis generally, but no numerical yield or batch scale beyond reagent amounts is given.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCopper(I) iodide5 mmol1678-1679 · 2.2 / 3.1 · Figure 1
LinkerTCNQnot reported for Cu route1678-1679 · 2.2 / 3.1 · Figure 1
SolventAcetonitrile100 mL1678-1679 · 2.2 / 3.1 · Figure 1
OtherEthanol washNot specified1678-1679 · 2.2 / 3.1 · Figure 1
Partial recipeSource: Main

Route 2: Hydrothermal

1678-1679 · 2.2 / 3.1

Metal precursorsIron acetate (AR, >=99%), 20 mmol
Linker precursorsTCNQ, 20 mmol
SolventsDMF, 60 mL
Atmosphereair/not specified
Temperature150
Time10 by methods; 6 in results discussion
Oxidant / reductantNot specified
Work-upSonicated 20 min, autoclaved, negative-pressure filtered, washed with DMF several times, dried at 65 deg C overnight.
ActivationNo activation reported beyond drying at 65 deg C overnight.
Scalability contextNo yield reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceIron acetate20 mmol1678-1679 · 2.2 / 3.1
LinkerTCNQ20 mmol1678-1679 · 2.2 / 3.1
SolventDMF60 mL1678-1679 · 2.2 / 3.1
Vague recipeSource: Main

Route 3: Other

1678 · 2.3

Metal precursorsPre-synthesised M-TCNQ powders
AdditivesParaffin matrix
Atmospherenot specified
Work-upPrepared for concentric-ring VNA testing at 50 wt% M-TCNQ loading; mixing/pressing details not reported.
Scalability contextApplication-composite preparation details are sparse.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherM-TCNQ complex50 wt% loading1678 · 2.3
AdditiveParaffinbalance1678 · 2.3
Partial recipeSource: Main

Route 4: Hydrothermal

1678-1679 · 2.2 / 3.1

Metal precursorsNickel acetate tetrahydrate (AR, >=99.5%), 20 mmol
Linker precursorsTCNQ, 20 mmol
SolventsDMF, 60 mL
Atmosphereair/not specified
Temperature150
Time10 by methods; 6 in results discussion
Oxidant / reductantNot specified
Work-upSonicated 20 min, autoclaved, negative-pressure filtered, washed with DMF several times, dried at 65 deg C overnight.
ActivationNo activation reported beyond drying at 65 deg C overnight.
Scalability contextNo yield reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNickel acetate tetrahydrate20 mmol1678-1679 · 2.2 / 3.1
LinkerTCNQ20 mmol1678-1679 · 2.2 / 3.1
SolventDMF60 mL1678-1679 · 2.2 / 3.1