Synthesis evidence

Stacked conductive metal–organic framework nanorods for high-performance vacuum electronic devices

Guan Z., Li J., Wu H. et al. · Ceramics International · 2022 · 34092-34097

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: Other

2 / p002 · Experimental section · Figure 4a inset

AdditivesDouble-sided conductive adhesive; FTO glass; phosphor coating on FTO anode
AtmosphereAssembly atmosphere not reported; field-emission testing was under high vacuum (~1 x 10-4 Pa) at room temperature.
Substrate orientationCu-CAT@GP cathode opposite phosphor-coated FTO anode
Work-upGlue coated graphite paper to FTO glass with double-sided conductive adhesive; assemble field-emission device.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Additivedouble-sided conductive adhesiveNot specified2 / p002 · Experimental section · Figure 4a inset
Otherfluorine-doped tin oxide (FTO) glassNot specified2 / p002 · Experimental section · Figure 4a inset
Otherphosphor coating on FTO anodeNot specified2 / p002 · Experimental section · Figure 4a inset
Complete recipeSource: Both

Route 2: Hydrothermal

2 / p002 · Experimental section · Figure 1a

Metal precursorsCopper acetate monohydrate (12 mg, 0.06 mmol)
Linker precursorsHHTP (2,3,6,7,10,11-Hexahydroxytriphenylene) (9.8 mg, 0.03 mmol)
Solvents1 mL deionized water/DMF (N,N-dimethylformamide), v:v = 1:1
AdditivesPretreated graphite paper substrate
AtmosphereReaction atmosphere not reported; pretreatment used vacuum oven drying and final freeze-drying used vacuum under 2 Pa.
Temperature85
Time24
Substrate orientationGraphite paper submerged in reactant solution; orientation not reported
Work-upCool reactor to room temperature; wash MOF-nanorod-coated graphite paper with deionized water three times; freeze washed product for 2 h at -70 deg C in the cold trap; transfer quickly to vacuum drying rack for 24 h under 2 Pa.
ActivationFreeze-drying: -70 deg C cold trap for 2 h followed by vacuum drying for 24 h under <2 Pa.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate monohydrate12 mg, 0.06 mmol2 / p002 · Experimental section · Figure 1a
LinkerHHTP (2,3,6,7,10,11-Hexahydroxytriphenylene)9.8 mg, 0.03 mmol2 / p002 · Experimental section · Figure 1a
Solventdeionized water/DMF (N,N-Dimethylformamide)1 mL; v:v = 1:12 / p002 · Experimental section · Figure 1a
Additivegraphite paperNot specified2 / p002 · Experimental section · Figure 1a
Partial recipeSource: Both

Route 3: Hydrothermal

3 / p003 · Results and discussion · Figure S1

Metal precursorsCopper acetate monohydrate (12 mg, 0.06 mmol), same as main 24 h route
Linker precursorsHHTP (2,3,6,7,10,11-Hexahydroxytriphenylene) (9.8 mg, 0.03 mmol), same as main 24 h route
Solvents1 mL deionized water/DMF (N,N-dimethylformamide), v:v = 1:1
AdditivesPretreated graphite paper substrate
AtmosphereReaction atmosphere not reported
Temperature85
Time3, 5, 7
Substrate orientationGraphite paper submerged in reactant solution; orientation not reported
Work-upWorkup for the time-series samples is not separately stated; main 24 h route was washed with deionized water and freeze-dried.
ActivationNot separately stated for the time-series SEM samples
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper acetate monohydrate12 mg, 0.06 mmol3 / p003 · Results and discussion · Figure S1
LinkerHHTP (2,3,6,7,10,11-Hexahydroxytriphenylene)9.8 mg, 0.03 mmol3 / p003 · Results and discussion · Figure S1
Solventdeionized water/DMF (N,N-Dimethylformamide)1 mL; v:v = 1:13 / p003 · Results and discussion · Figure S1
Additivegraphite paperNot specified3 / p003 · Results and discussion · Figure S1
Complete recipeSource: SI

Route 4: Other

text-only SI · Experimental section - Pretreatment of graphite paper

SolventsDeionized water / acetone / isopropanol (v = 1:1:1); ethanol wash
AdditivesGraphite paper
AtmosphereVacuum oven for drying; cleaning atmosphere otherwise not reported
Temperature100
Time0.5 h ultrasonic cleaning; 6 h drying
Substrate orientationNot reported
Work-upUltrasonically clean graphite paper in deionized water/acetone/isopropanol (1:1:1) for 30 min, wash with ethanol three times, then dry at 100 deg C under vacuum for 6 h.
ActivationVacuum drying at 100 deg C for 6 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Othergraphite paperNot specifiedtext-only SI · Experimental section - Pretreatment of graphite paper
Solventdeionized water / acetone / isopropanolv = 1:1:1text-only SI · Experimental section - Pretreatment of graphite paper
Solventethanolwashed 3 timestext-only SI · Experimental section - Pretreatment of graphite paper