Synthesis · Microwave discharge for rapid introduction of bimetallic-synergistic configuration to conductive catecholate toward long-term supercapacitor

9 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2 · 2.2. Synthesis of Ni-CAT

Metal precursors10 mg Ni(OAc)2.4H2O

Linker precursors7 mg HHTP

Solvents4 mL deionized water; deionized water and anhydrous ethanol for rinsing

AdditivesConcentrated hydrochloric acid used to pretreat carbon cloth

Atmospherenot specified for Ni-CAT growth

Temperature60

Time4 h growth after 4 h acid pretreatment; 12 h drying

Substrate orientationPretreated carbon cloth immersed in precursor solution

Work-upAfter cooling to room temperature within 1 h, rinsed three times with deionized water and anhydrous ethanol.

ActivationVacuum drying oven at 60 C for 12 h

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	carbon cloth (CC)	1 cm x 2 cm	2 · 2.2. Synthesis of Ni-CAT
Acid	concentrated hydrochloric acid	10 mL · concentrated	2 · 2.2. Synthesis of Ni-CAT
Metal Source	nickel acetate tetrahydrate (Ni(OAc)2.4H2O)	10 mg	2 · 2.2. Synthesis of Ni-CAT
Linker	2,3,6,7,10,11-hexahydroxy triphenyl (HHTP)	7 mg	2 · 2.2. Synthesis of Ni-CAT
Solvent	deionized water	4 mL	2 · 2.2. Synthesis of Ni-CAT

Complete recipeSource: Main

Route 2: Other

2 · 2.5. Preparation of the symmetrical Solid-State supercapacitor

Metal precursorsZn,Ni-CAT electrode

SolventsWater for PVA/KCl gel electrolyte

Additives4 g PVA powder; 3 M KCl

AtmosphereDevice sealed to prevent moisture from air

Temperature85 for gel preparation; room temperature drying

Time30 min electrode immersion in gel; 30 min drying at room temperature

Substrate orientationSymmetric two-electrode structure using Zn,Ni-CAT as both electrodes

Work-upAssembled device sealed

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Electrolyte	PVA powder	4 g	2 · 2.5. Preparation of the symmetrical Solid-State supercapacitor
Electrolyte	KCl water	40 mL · 3 M KCl	2 · 2.5. Preparation of the symmetrical Solid-State supercapacitor
Other	Zn,Ni-CAT electrode	Not specified	2 · 2.5. Preparation of the symmetrical Solid-State supercapacitor

Partial recipeSource: Both

Route 3: Other

6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7

Metal precursorsPrepared Ni-CAT and zinc wire

Linker precursorsHHTP-derived linker already present in Ni-CAT

SolventsDilute acid and deionized water for post-treatment

AtmosphereAr gas purged for 10 min before microwave reaction

Temperaturenot directly specified for over-treatment sample; pulse-series temperature profile reaches 649.2 C in 4 s

Time25 s total microwave treatment

Substrate orientationNi-CAT placed at bottom of quartz container; zinc wire fixed 20 mm above sample

Work-upTreated by dilute acid and deionized water after reaction, by analogy to the T1-T4 pulse route.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	prepared Ni-CAT on carbon cloth	1 cm x 2 cm sample implied	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7
Metal Source	zinc wire	fixed 20 mm above the sample	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7
Other	argon	pumped for 10 min · 99.9 % purity	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7

Partial recipeSource: Both

Route 4: Other

6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7

Metal precursorsPrepared Ni-CAT and zinc wire

Linker precursorsHHTP-derived linker already present in Ni-CAT

SolventsDilute acid and deionized water for post-treatment

AtmosphereAr gas purged for 10 min before microwave reaction

Temperaturenot directly specified for over-treatment sample; pulse-series temperature profile reaches 649.2 C in 4 s

Time60 s total microwave treatment

Substrate orientationNi-CAT placed at bottom of quartz container; zinc wire fixed 20 mm above sample

Work-upTreated by dilute acid and deionized water after reaction, by analogy to the T1-T4 pulse route.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	prepared Ni-CAT on carbon cloth	1 cm x 2 cm sample implied	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7
Metal Source	zinc wire	fixed 20 mm above the sample	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7
Other	argon	pumped for 10 min · 99.9 % purity	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figures S6-S7

Complete recipeSource: Main

Route 5: Solvothermal

2 · 2.4. Synthesis of Zn,Ni-CAT-Solvothermal

Metal precursors0.15 mmol nickel acetate hexahydrate; 0.15 mmol zinc acetate

Linker precursors0.15 mmol HHTP

Solvents5 mL water-DMF solvent mixture, volume ratio 1:1

Atmospherenot specified

Temperature85

Time10 h heat; 10 min sonication; cooled to room temperature within 30 min; dried overnight at 60 C

Substrate orientationPretreated carbon cloth (1 cm x 2 cm) immersed in reaction solution

Work-upWashed thoroughly with deionized water

ActivationDried overnight at 60 C

Scalability contextComparison conventional route is much longer than 20 s microwave route.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel acetate hexahydrate	0.15 mmol	2 · 2.4. Synthesis of Zn,Ni-CAT-Solvothermal
Metal Source	zinc acetate	0.15 mmol	2 · 2.4. Synthesis of Zn,Ni-CAT-Solvothermal
Linker	HHTP	0.15 mmol	2 · 2.4. Synthesis of Zn,Ni-CAT-Solvothermal
Solvent	water-DMF	5 mL · volume ratio = 1:1	2 · 2.4. Synthesis of Zn,Ni-CAT-Solvothermal
Other	pretreated CC	1 cm x 2 cm	2 · 2.4. Synthesis of Zn,Ni-CAT-Solvothermal

Complete recipeSource: Main

Route 6: Other

2 · 2.3. Synthesis of Zn,Ni-CAT

Metal precursorsPrepared Ni-CAT and zinc wire

Linker precursorsHHTP-derived linker already present in Ni-CAT

SolventsDilute acid and deionized water for post-treatment

AtmosphereAr gas purged for 10 min to ensure an oxygen-free environment

TemperatureReal-time pulse temperature reported separately; single pulse reaches 649.2 C in 4 s in Figure 4a

Time5 s microwave pulse

Substrate orientationNi-CAT placed at bottom of quartz container; zinc wire fixed 20 mm above sample; bottom Ni-CAT side aligned with temperature detector

Oxidant / reductantHigh-energy Zn particles generated from Zn wire by microwave pulse-induced plasma/arc

Work-upTreated by dilute acid and deionized water after reaction

Scalability contextAuthors describe the strategy as rapid, acid/base-free and generic, with a 5 s pulse for T1.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	prepared Ni-CAT	Not specified	2 · 2.3. Synthesis of Zn,Ni-CAT
Metal Source	zinc wire	fixed 20 mm above the sample	2 · 2.3. Synthesis of Zn,Ni-CAT
Other	argon	pumped for 10 min · 99.9% purity	2 · 2.3. Synthesis of Zn,Ni-CAT

Complete recipeSource: Main

Route 7: Other

2 · 2.3. Synthesis of Zn,Ni-CAT

Metal precursorsPrepared Ni-CAT and zinc wire

Linker precursorsHHTP-derived linker already present in Ni-CAT

SolventsDilute acid and deionized water for post-treatment

AtmosphereAr gas purged for 10 min

TemperaturePulse temperature profile shown in Figure 4a

Time10 s total microwave treatment, two 5 s pulses

Substrate orientationNi-CAT at bottom of quartz container; zinc wire 20 mm above sample

Oxidant / reductantMicrowave pulse-induced plasma/arc generating active Zn particles

Work-upTreated by dilute acid and deionized water after reaction

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	prepared Ni-CAT	Not specified	2 · 2.3. Synthesis of Zn,Ni-CAT
Metal Source	zinc wire	fixed 20 mm above the sample	2 · 2.3. Synthesis of Zn,Ni-CAT
Other	argon	pumped for 10 min · 99.9% purity	2 · 2.3. Synthesis of Zn,Ni-CAT

Complete recipeSource: Main

Route 8: Other

6 · 3.3. Optimization of bimetallic MOFs by microwave · Figure 4

Metal precursorsPrepared Ni-CAT and zinc wire

Linker precursorsHHTP-derived linker already present in Ni-CAT

SolventsDilute acid and deionized water for post-treatment

AtmosphereAr gas purged for 10 min

TemperaturePulse temperature profile shown in Figure 4a

Time15 s total microwave treatment, three 5 s pulses

Substrate orientationNi-CAT at bottom of quartz container; zinc wire 20 mm above sample

Oxidant / reductantMicrowave pulse-induced plasma/arc generating active Zn particles

Work-upTreated by dilute acid and deionized water after reaction

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	prepared Ni-CAT	Not specified	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figure 4
Metal Source	zinc wire	fixed 20 mm above the sample	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figure 4
Other	argon	pumped for 10 min · 99.9% purity	6 · 3.3. Optimization of bimetallic MOFs by microwave · Figure 4

Complete recipeSource: Main

Route 9: Other

2 · 2.3. Synthesis of Zn,Ni-CAT

Metal precursorsPrepared Ni-CAT and zinc wire

Linker precursorsHHTP-derived linker already present in Ni-CAT

SolventsDilute acid and deionized water for post-treatment

AtmosphereAr gas purged for 10 min to ensure an oxygen-free environment

TemperatureReal-time pulse temperature up to 649.2 C within 4 s; rapid cooling by 250 C within 1 s when pulse suspended

Time20 s total microwave treatment, four 5 s pulses

Substrate orientationNi-CAT placed at bottom of quartz container; zinc wire fixed 20 mm above sample; bottom Ni-CAT side aligned with temperature detector

Oxidant / reductantHigh-energy zinc particles generated from Zn wire by microwave pulse-induced plasma and arc

Work-upTreated by dilute acid and deionized water after reaction

Scalability context20 s route claimed as rapid and scalable in the conclusion.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	prepared Ni-CAT	Not specified	2 · 2.3. Synthesis of Zn,Ni-CAT
Metal Source	zinc wire	fixed 20 mm above the sample	2 · 2.3. Synthesis of Zn,Ni-CAT
Other	argon	pumped for 10 min · 99.9% purity	2 · 2.3. Synthesis of Zn,Ni-CAT
Acid	dilute acid	dilute; exact identity not specified	2 · 2.3. Synthesis of Zn,Ni-CAT