Synthesis · Radiation-Induced in Situ Construction of 2D Conductive Defect-Rich Metal-Organic Frameworks for High-Performance Supercapacitor

5 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

Section S1-S2

Metal precursorsCu(OAc)2 / Cu(CH3COO)2; SI gives 0.53 mmol (0.127 g)

Linker precursorsHHTP; SI gives 4 mmol (0.13 g), internally inconsistent with HHTP molar mass

SolventsMain text: DMF and NH3.H2O; SI: 10 mL water/ammonium hydroxide mixed solution (v/v = 9:1)

AdditivesAmmonium hydroxide / NH3.H2O

AtmosphereNitrogen injected for 20 min to remove air before irradiation

Temperatureambient during irradiation; dried at 60 degC after washing

Time17

Oxidant / reductant60Co gamma radiation; radiolysis generates solvated electrons, H radicals and OH radicals; absorbed dose 100 kGy

Work-upWashed with DMF and ethanol; dried at 60 degC

ActivationDried at 60 degC; no separate activation reported

Scalability contextAmbient-condition radiation route; irradiation facility activity 12000-13500 Ci and highest absorbed dose rate 30 Gy min-1 reported in SI.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	2,3,6,7,10,11-Hexahydroxytriphenylene hydrate (HHTP)	4 mmol (0.13 g)	Section S1-S2
Metal Source	Copper(II) acetate monohydrate / Cu(OAc)2	0.53 mmol (0.127 g)	Section S1-S2
Solvent	water/ammonium hydroxide mixed solution	10 mL · v/v = 9:1	Section S1-S2
Solvent	DMF	used in main-text precursor mixture and workup wash	Section S1-S2
Additive	ammonium hydroxide / NH3.H2O	part of 10 mL mixed solution	Section S1-S2

Partial recipeSource: Both

Route 2: Hydrothermal

Section S1

Metal precursorsSame solution formula as Cu-CAT-Rad: Cu(OAc)2 / Cu(CH3COO)2; SI gives 0.53 mmol (0.127 g)

Linker precursorsSame solution formula as Cu-CAT-Rad: HHTP; SI gives 4 mmol (0.13 g)

SolventsSame solution formula as Cu-CAT-Rad: main text says DMF and NH3.H2O; SI says 10 mL water/ammonium hydroxide (v/v = 9:1)

AdditivesAmmonium hydroxide / NH3.H2O

AtmosphereNot stated for hydrothermal step; same solution formula implies preparation as above but not explicitly degassed

Temperature85

Time24

Oxidant / reductantNone reported; conventional hydrothermal/solvothermal control

Work-upNot separately stated for Cu-CAT-Sol; likely same post-wash not explicit

ActivationNot explicitly reported

Scalability contextConventional thermal comparison sample.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	same as Cu-CAT-Rad: 4 mmol (0.13 g)	Section S1
Metal Source	Cu(OAc)2	same as Cu-CAT-Rad: 0.53 mmol (0.127 g)	Section S1
Solvent	water/ammonium hydroxide mixed solution	same as Cu-CAT-Rad: 10 mL · v/v = 9:1	Section S1

Vague recipeSource: Both

Route 3: Other

Section S1

Metal precursorsCu-CAT-Rad electrodes

Linker precursorsAlready incorporated in Cu-CAT-Rad

Solvents3.0 M KCl electrolyte

AtmosphereNot stated

Substrate orientationSymmetric two-electrode button-cell assembly

Work-upDevice assembled with Cu-CAT-Rad as cathode and anode

ActivationNo activation reported

Scalability contextTwo series-connected devices powered five 2.0 V green LEDs.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-CAT-Rad	used as cathode and anode	Section S1
Electrolyte	KCl	not reported · 3.0 M	Section S1

Partial recipeSource: SI

Route 4: Drop Cast

Section S1

Metal precursorsCu-CAT-Rad powder

Linker precursorsAlready incorporated in Cu-CAT-Rad powder

SolventsN-methyl pyrrolidone (NMP)

AdditivesAcetylene black; PVDF binder

AtmosphereNot stated

Temperature60

Timeovernight drying

Substrate orientationNi foam substrate

Work-upSlurry coated on Ni foam and dried at 60 degC overnight

ActivationNo separate activation reported

Scalability contextMass loading about 3 mg cm-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-CAT-Rad	8 parts by mass in 8:1:1 mixture	Section S1
Additive	acetylene black	1 part by mass	Section S1
Additive	PVDF	1 part by mass	Section S1
Solvent	N-methyl pyrrolidone (NMP)	not reported	Section S1

Partial recipeSource: SI

Route 5: Drop Cast

Section S1

Metal precursorsCu-CAT-Sol powder

Linker precursorsAlready incorporated in Cu-CAT-Sol powder

SolventsN-methyl pyrrolidone (NMP)

AdditivesAcetylene black; PVDF binder

AtmosphereNot stated

Temperature60

Timeovernight drying

Substrate orientationNi foam substrate

Work-upSlurry coated on Ni foam and dried at 60 degC overnight

ActivationNo separate activation reported

Scalability contextMass loading about 3 mg cm-2.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Cu-CAT-Sol	8 parts by mass in 8:1:1 mixture	Section S1
Additive	acetylene black	1 part by mass	Section S1
Additive	PVDF	1 part by mass	Section S1
Solvent	NMP	not reported	Section S1