Synthesis · Successful In Situ Growth of Conductive MOFs on 2D Cobalt-Based Compounds and Their Electrochemical Performance

22 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

SI p. 9 · Chemicals and synthesis

Metal precursorspre-synthesized Co(OH)2, 30 mg

Atmosphereair

Temperature270

Time1

Substrate orientationtube furnace

Oxidant / reductantcalcination/oxidation in air

Work-upproduct collected after cooling

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	30 mg	SI p. 9 · Chemicals and synthesis

Complete recipeSource: SI

Route 2: Solvothermal

SI p. 5 · Chemicals and synthesis · Table S1

Metal precursorsCo(CH3COO)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound until uniformly dispersed

Atmospherenot specified

Temperature85

Time12

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	7 mg	SI p. 5 · Chemicals and synthesis · Table S1
Metal Source	Co(CH3COO)2.4H2O	10 mg	SI p. 5 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 5 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 3: Solvothermal

SI p. 9-10 · Chemicals and synthesis · Table S3

Metal precursorsCo(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized Co3O4

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co3O4	10 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Metal Source	Co(OAc)2.4H2O	10 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Linker	HHTP	7 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Solvent	deionized water	4 mL	SI p. 9-10 · Chemicals and synthesis · Table S3

Complete recipeSource: SI

Route 4: Solvothermal

SI p. 9-10 · Chemicals and synthesis · Table S3

Metal precursorsCo(OAc)2.4H2O

Linker precursorsHHTP, 3.5 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation5 mg pre-synthesized Co3O4

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co3O4	5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Metal Source	Co(OAc)2.4H2O	5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Linker	HHTP	3.5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Solvent	deionized water	4 mL	SI p. 9-10 · Chemicals and synthesis · Table S3

Complete recipeSource: SI

Route 5: Solvothermal

SI p. 6-7 · Chemicals and synthesis · Table S1

Metal precursorsCo(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized Co(OH)2

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	10 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Metal Source	Co(OAc)2.4H2O	10 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Linker	HHTP	7 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 6-7 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 6: Solvothermal

SI p. 6-7 · Chemicals and synthesis · Table S1

Metal precursorsCo(OAc)2.4H2O

Linker precursorsHHTP, 3.5 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation5 mg pre-synthesized Co(OH)2

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Metal Source	Co(OAc)2.4H2O	5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Linker	HHTP	3.5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 6-7 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 7: Solvothermal

SI p. 7-9 · Chemicals and synthesis · Table S2

Metal precursorsCo(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized CoP

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized CoP	10 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Metal Source	Co(OAc)2.4H2O	10 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Linker	HHTP	7 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Solvent	deionized water	4 mL	SI p. 7-9 · Chemicals and synthesis · Table S2

Complete recipeSource: SI

Route 8: Solvothermal

SI p. 7-9 · Chemicals and synthesis · Table S2

Metal precursorsCo(OAc)2.4H2O

Linker precursorsHHTP, 3.5 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation5 mg pre-synthesized CoP

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized CoP	5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Metal Source	Co(OAc)2.4H2O	5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Linker	HHTP	3.5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Solvent	deionized water	4 mL	SI p. 7-9 · Chemicals and synthesis · Table S2

Complete recipeSource: SI

Route 9: Hydrothermal

SI p. 5 · Chemicals and synthesis

Metal precursorsCo(CH3COO)2.4H2O, 0.6974 g

Solvents0.05 M aluminum chloride solution, 20 mL

Additivesammonia solution 25%, 2 mL

Atmospheresealed autoclave

Temperature120

Time6

Oxidant / reductantammonia base

Work-upcentrifuged at 6000 rpm for 1 min; washed with deionized water and ethanol; centrifuged three times

Activationdried in air under ambient conditions

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Co(CH3COO)2.4H2O	0.6974 g	SI p. 5 · Chemicals and synthesis
Additive	AlCl3 aqueous solution	20 mL · 0.05 M	SI p. 5 · Chemicals and synthesis
Base	ammonia solution	2 mL · 25%	SI p. 5 · Chemicals and synthesis

Complete recipeSource: SI

Route 10: Other

SI p. 7 · Chemicals and synthesis

Metal precursorspre-synthesized Co(OH)2, 30 mg

Solventsdeionized water after phosphorization

AdditivesNaH2PO2.H2O, 300 mg

AtmosphereN2

Temperature430

Time1

Substrate orientationCo(OH)2 downstream; NaH2PO2.H2O upstream in tube furnace

Oxidant / reductantphosphorization by NaH2PO2.H2O

Work-upcooled sample sonicated in deionized water for 30 min; collected after centrifuging and sonicating

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	30 mg	SI p. 7 · Chemicals and synthesis
Reductant	NaH2PO2.H2O	300 mg	SI p. 7 · Chemicals and synthesis
Solvent	deionized water	certain amount	SI p. 7 · Chemicals and synthesis

Complete recipeSource: SI

Route 11: Solvothermal

SI p. 5 · Chemicals and synthesis · Table S1

Metal precursorsNi(CH3COO)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound until uniformly dispersed

Atmospherenot specified

Temperature85

Time12

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	7 mg	SI p. 5 · Chemicals and synthesis · Table S1
Metal Source	Ni(CH3COO)2.4H2O	10 mg	SI p. 5 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 5 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 12: Solvothermal

SI p. 9-10 · Chemicals and synthesis · Table S3

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized Co3O4

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co3O4	10 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Metal Source	Ni(OAc)2.4H2O	10 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Linker	HHTP	7 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Solvent	deionized water	4 mL	SI p. 9-10 · Chemicals and synthesis · Table S3

Complete recipeSource: SI

Route 13: Solvothermal

SI p. 9-10 · Chemicals and synthesis · Table S3

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP, 3.5 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation5 mg pre-synthesized Co3O4

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co3O4	5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Metal Source	Ni(OAc)2.4H2O	5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Linker	HHTP	3.5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Solvent	deionized water	4 mL	SI p. 9-10 · Chemicals and synthesis · Table S3

Complete recipeSource: SI

Route 14: Solvothermal

SI p. 6-7 · Chemicals and synthesis · Table S1

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized Co(OH)2

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	10 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Metal Source	Ni(OAc)2.4H2O	10 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Linker	HHTP	7 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 6-7 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 15: Other

SI p. 12 · Asymmetric supercapacitor assembly and measurements

Metal precursorsNi-HHTP@Co(OH)2 positive electrode

Solvents3 M KOH electrolyte

Additivesactivated carbon YEC-8; acetylene black; PTFE

Atmosphereambient aqueous cell

Substrate orientationnickel foam electrodes

Work-uppositive and negative powders coated on nickel foam and pressed at 8 MPa

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-HHTP@Co(OH)2	about 2 mg loading	SI p. 12 · Asymmetric supercapacitor assembly and measurements
Other	activated carbon YEC-8	about 2 mg active material in SI; 7.45 mg loading in main text	SI p. 12 · Asymmetric supercapacitor assembly and measurements
Additive	acetylene black	Not specified	SI p. 12 · Asymmetric supercapacitor assembly and measurements
Additive	polytetrafluoroethylene	Not specified	SI p. 12 · Asymmetric supercapacitor assembly and measurements
Electrolyte	KOH	3 M	SI p. 12 · Asymmetric supercapacitor assembly and measurements

Complete recipeSource: SI

Route 16: Solvothermal

SI p. 6-7 · Chemicals and synthesis · Table S1

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP, 3.5 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation5 mg pre-synthesized Co(OH)2

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Metal Source	Ni(OAc)2.4H2O	5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Linker	HHTP	3.5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 6-7 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 17: Solvothermal

SI p. 7-9 · Chemicals and synthesis · Table S2

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized CoP

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized CoP	10 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Metal Source	Ni(OAc)2.4H2O	10 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Linker	HHTP	7 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Solvent	deionized water	4 mL	SI p. 7-9 · Chemicals and synthesis · Table S2

Complete recipeSource: SI

Route 18: Solvothermal

SI p. 7-9 · Chemicals and synthesis · Table S2

Metal precursorsNi(OAc)2.4H2O

Linker precursorsHHTP, 3.5 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation5 mg pre-synthesized CoP

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized CoP	5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Metal Source	Ni(OAc)2.4H2O	5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Linker	HHTP	3.5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Solvent	deionized water	4 mL	SI p. 7-9 · Chemicals and synthesis · Table S2

Complete recipeSource: SI

Route 19: Solvothermal

SI p. 5 · Chemicals and synthesis · Table S1

Metal precursorsNi(CH3COO)2.4H2O + Co(CH3COO)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound until uniformly dispersed

Atmospherenot specified

Temperature85

Time12

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	HHTP	7 mg	SI p. 5 · Chemicals and synthesis · Table S1
Metal Source	Ni(CH3COO)2.4H2O + Co(CH3COO)2.4H2O	5 mg + 5 mg	SI p. 5 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 5 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 20: Solvothermal

SI p. 9-10 · Chemicals and synthesis · Table S3

Metal precursorsNi(OAc)2.4H2O + Co(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized Co3O4

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co3O4	10 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Metal Source	Ni(OAc)2.4H2O + Co(OAc)2.4H2O	5 mg + 5 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Linker	HHTP	7 mg	SI p. 9-10 · Chemicals and synthesis · Table S3
Solvent	deionized water	4 mL	SI p. 9-10 · Chemicals and synthesis · Table S3

Complete recipeSource: SI

Route 21: Solvothermal

SI p. 6-7 · Chemicals and synthesis · Table S1

Metal precursorsNi(OAc)2.4H2O + Co(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized Co(OH)2

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized Co(OH)2	10 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Metal Source	Ni(OAc)2.4H2O + Co(OAc)2.4H2O	5 mg + 5 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Linker	HHTP	7 mg	SI p. 6-7 · Chemicals and synthesis · Table S1
Solvent	deionized water	4 mL	SI p. 6-7 · Chemicals and synthesis · Table S1

Complete recipeSource: SI

Route 22: Solvothermal

SI p. 7-9 · Chemicals and synthesis · Table S2

Metal precursorsNi(OAc)2.4H2O + Co(OAc)2.4H2O

Linker precursorsHHTP, 7 mg

Solventsdeionized water, 4 mL

Additivesultrasound 15 min before HHTP addition and 15 min after

Atmospherenot specified

Temperature85

Time12

Substrate orientation10 mg pre-synthesized CoP

Work-upwashed with deionized water and acetone; centrifuged three times

Activationdried at room temperature overnight

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	pre-synthesized CoP	10 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Metal Source	Ni(OAc)2.4H2O + Co(OAc)2.4H2O	5 mg + 5 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Linker	HHTP	7 mg	SI p. 7-9 · Chemicals and synthesis · Table S2
Solvent	deionized water	4 mL	SI p. 7-9 · Chemicals and synthesis · Table S2