Synthesis · Enhanced conductivity and energy storing performances of 3D bimetallic conductive metal-organic frameworks based on linear π-conjugated thiazole for supercapacitors

8 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Hydrothermal

2 · 2.2

Metal precursorsCo(NO3)2.6H2O (7.85 mg, 0.027 mmol)

Linker precursorsBDC (4.98 mg, 0.03 mmol); DPTTZ (7.4 mg, 0.025 mmol)

Solventsdeionised water (0.5 mL) and DMF (2 mL)

Atmospherenot stated

Temperature120

Time24

Work-upcentrifugation; washed sequentially with water and DMF

Activationvacuum dried at 80 C for 12 h

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	7.85 mg, 0.027 mmol	2 · 2.2
Linker	BDC	4.98 mg, 0.03 mmol	2 · 2.2
Linker	DPTTZ	7.4 mg, 0.025 mmol	2 · 2.2
Solvent	deionized water	0.5 mL	2 · 2.2
Solvent	DMF	2 mL	2 · 2.2

Partial recipeSource: Both

Route 2: Other

2 · 2.1 · Fig. 1a; Scheme S1 referenced

Metal precursorsnone

Linker precursors4-picolinic acid (0.4 mL) and dithiourea (200 mg); section text also describes pyridinecarboxaldehyde and dithiooxamide

SolventsDMF (10 mL)

Atmosphereambient environment described for the condensation; no inert gas stated

Temperature153

Time5

Work-upcooled to ambient temperature using an ice bath; isolated by filtration; washed thoroughly with deionised water

Activationdried under reduced pressure

Scalability contextAuthors describe the DPTTZ synthesis as straightforward and in an ambient environment.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	4-picolinic acid	0.4 mL	2 · 2.1 · Fig. 1a; Scheme S1 referenced
Linker	dithiourea	200 mg	2 · 2.1 · Fig. 1a; Scheme S1 referenced
Solvent	DMF	10 mL	2 · 2.1 · Fig. 1a; Scheme S1 referenced

Partial recipeSource: Both

Route 3: Hydrothermal

3 · 2.3

Metal precursorsCo(NO3)2.6H2O and Ni(NO3)2.6H2O, x:y = 1:1, total metal ions 0.027 mmol

Linker precursorsBDC (4.98 mg, 0.03 mmol); DPTTZ (7.4 mg, 0.025 mmol)

SolventsDMF (2 mL) and water (0.5 mL)

Atmospherenot stated

Temperature120

Time24

Work-upobtained products after hydrothermal reaction; detailed washing/drying not repeated for bimetallic route

Activationnot stated in bimetallic subsection

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of total metal ions 0.027 mmol, x:y = 1:1	3 · 2.3
Metal Source	Ni(NO3)2.6H2O	part of total metal ions 0.027 mmol, x:y = 1:1	3 · 2.3
Linker	BDC	4.98 mg, 0.03 mmol	3 · 2.3
Linker	DPTTZ	7.4 mg, 0.025 mmol	3 · 2.3
Solvent	DMF	2 mL	3 · 2.3
Solvent	water	0.5 mL	3 · 2.3

Partial recipeSource: Both

Route 4: Hydrothermal

3 · 2.3

Metal precursorsCo(NO3)2.6H2O and Ni(NO3)2.6H2O, x:y = 1:3, total metal ions 0.027 mmol

Linker precursorsBDC (4.98 mg, 0.03 mmol); DPTTZ (7.4 mg, 0.025 mmol)

SolventsDMF (2 mL) and water (0.5 mL)

Atmospherenot stated

Temperature120

Time24

Work-upobtained products after hydrothermal reaction; detailed washing/drying not repeated for bimetallic route

Activationnot stated in bimetallic subsection

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of total metal ions 0.027 mmol, x:y = 1:3	3 · 2.3
Metal Source	Ni(NO3)2.6H2O	part of total metal ions 0.027 mmol, x:y = 1:3	3 · 2.3
Linker	BDC	4.98 mg, 0.03 mmol	3 · 2.3
Linker	DPTTZ	7.4 mg, 0.025 mmol	3 · 2.3
Solvent	DMF	2 mL	3 · 2.3
Solvent	water	0.5 mL	3 · 2.3

Partial recipeSource: Both

Route 5: Other

3 · 2.5 · Fig. S25 referenced

Metal precursorsNi3Co1-DPTTZ-MOF positive electrode

Solvents3.0 M KOH electrolyte

Additivesactivated carbon negative electrode; glass microfiber filter separator

Atmospherenot stated

Work-upassembled as asymmetric supercapacitor with mass ratio positive:negative = 1:1.6

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni3Co1-DPTTZ-MOF positive electrode	active mass < 1 mg cm-2 for cathode in device section	3 · 2.5 · Fig. S25 referenced
Other	activated carbon negative electrode	mass ratio positive:negative = 1:1.6	3 · 2.5 · Fig. S25 referenced
Electrolyte	KOH	3.0 M	3 · 2.5 · Fig. S25 referenced

Partial recipeSource: Both

Route 6: Hydrothermal

3 · 2.3

Metal precursorsCo(NO3)2.6H2O and Ni(NO3)2.6H2O, x:y = 3:1, total metal ions 0.027 mmol

Linker precursorsBDC (4.98 mg, 0.03 mmol); DPTTZ (7.4 mg, 0.025 mmol)

SolventsDMF (2 mL) and water (0.5 mL)

Atmospherenot stated

Temperature120

Time24

Work-upobtained products after hydrothermal reaction; detailed washing/drying not repeated for bimetallic route

Activationnot stated in bimetallic subsection

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(NO3)2.6H2O	part of total metal ions 0.027 mmol, x:y = 3:1	3 · 2.3
Metal Source	Ni(NO3)2.6H2O	part of total metal ions 0.027 mmol, x:y = 3:1	3 · 2.3
Linker	BDC	4.98 mg, 0.03 mmol	3 · 2.3
Linker	DPTTZ	7.4 mg, 0.025 mmol	3 · 2.3
Solvent	DMF	2 mL	3 · 2.3
Solvent	water	0.5 mL	3 · 2.3

Partial recipeSource: Both

Route 7: Hydrothermal

2 · 2.2

Metal precursorsNi(NO3)2.6H2O substituted for Co(NO3)2.6H2O; amount not independently stated

Linker precursorsBDC (4.98 mg, 0.03 mmol); DPTTZ (7.4 mg, 0.025 mmol)

Solventsdeionised water (0.5 mL) and DMF (2 mL)

Atmospherenot stated

Temperature120

Time24

Work-upsame as Co-DPTTZ-MOF: centrifugation, water/DMF washing

Activationsame as Co-DPTTZ-MOF: vacuum dried at 80 C for 12 h

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	substituted for Co(NO3)2.6H2O; amount not stated	2 · 2.2
Linker	BDC	4.98 mg, 0.03 mmol	2 · 2.2
Linker	DPTTZ	7.4 mg, 0.025 mmol	2 · 2.2
Solvent	deionized water	0.5 mL	2 · 2.2
Solvent	DMF	2 mL	2 · 2.2

Partial recipeSource: Both

Route 8: Other

3 · 2.4

Metal precursorspre-synthesised NiCo-DPTTZ-MOFs

Solventsisopropanol; PVDF dispersed in N-methyl pyrrolidone at 20 mg mL-1

Additivespolyvinylidene fluoride binder; Ketjen Black conductive agent

Atmospherenot stated

Temperature60

Timeovernight drying

Substrate orientation1 cm x 2 cm nickel foam

Work-upmixed at 80:15:5 active material:binder:conductive agent, ground to slurry, applied to nickel foam

Activationvacuum-dried at 60 C overnight; pressed at 10 MPa for 5 s

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NiCo-DPTTZ-MOFs active material	80 wt parts	3 · 2.4
Additive	polyvinylidene fluoride binder	15 wt parts · 20 mg mL-1 in N-methyl pyrrolidone	3 · 2.4
Additive	Ketjen Black conductive agent	5 wt parts	3 · 2.4
Solvent	isopropanol	Not specified	3 · 2.4