Synthesis · Conductive metal–Organic frameworks endow high-efficient oxygen evolution of La0·6Sr0·4Co0·8Fe0·2O3 perovskite oxide nanofibers

7 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

2 · 2.5 Electrode preparation

Metal precursors5.0 mg catalyst

Solvents500 uL isopropyl alcohol; 470 uL DI water

Additives1 mg conductive acetylene black; 30 uL Nafion solution (5.0 wt%)

Atmospheredried naturally in air

Substrate orientationglassy carbon disk electrode, 5 mm diameter, 0.196 cm2

Work-upInk ultrasonicated about 40 min; 10 uL dropped on glassy carbon electrode.

ActivationElectrochemical activation by CV scan at 50 mV s-1 for about 20 cycles before measurements.

Scalability contextElectrode loading 0.306 mg_total cm-2, 0.255 mg_oxide cm-2.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	catalyst	5.0 mg	2 · 2.5 Electrode preparation
Additive	conductive acetylene black	1 mg	2 · 2.5 Electrode preparation
Solvent	isopropyl alcohol	500 uL	2 · 2.5 Electrode preparation
Solvent	DI water	470 uL	2 · 2.5 Electrode preparation
Additive	Nafion solution	30 uL · 5.0 wt%	2 · 2.5 Electrode preparation

Complete recipeSource: Main

Route 2: Other

2 · 2.2 Preparation of LSCF NFs

Metal precursorsLa(NO3)3.6H2O (0.45 mmol); Sr(NO3)2 (0.3 mmol); Co(NO3)2.9H2O reported in route (0.6 mmol); Fe(NO3)9.9H2O reported in route (0.15 mmol); total metal ions 1.5 mmol

Solvents10 mL DMF

AdditivesPVP, 15 wt% based on mass of DMF

Atmosphereair during calcination

Temperature750

Time3

Work-upElectrospinning precursor solution through a 23-gauge needle at 0.01 mL min-1, 16 cm tip-collector distance, 16 kV, 30-40% relative humidity.

ActivationCalcination in air at 750 deg C for 3 h with heating rate 2 deg C min-1.

Scalability contextElectrospinning route uses controlled humidity, feed rate and voltage; no batch yield reported.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	La(NO3)3.6H2O	0.45 mmol	2 · 2.2 Preparation of LSCF NFs
Metal Source	Sr(NO3)2	0.3 mmol	2 · 2.2 Preparation of LSCF NFs
Metal Source	Co(NO3)2.9H2O	0.6 mmol	2 · 2.2 Preparation of LSCF NFs
Metal Source	Fe(NO3)9.9H2O	0.15 mmol	2 · 2.2 Preparation of LSCF NFs
Solvent	DMF	10 mL	2 · 2.2 Preparation of LSCF NFs
Additive	PVP	15 wt% based on mass of DMF	2 · 2.2 Preparation of LSCF NFs

Complete recipeSource: Main

Route 3: Solvothermal

2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Metal precursors20 mg LSCF NFs; 5 mg Ni(CH3COO)2.4H2O reported in comparison route

Linker precursors3.5 mg HATP.6HCl ligand

Solvents2 mL methanol; 1 mL DMF

Temperature70

Time3

Work-upLSCF dispersed by sonication for 20 min; ligand and nickel acetate added and sonicated for 10 min; product centrifuged and washed with DMF and ethanol.

ActivationDried under vacuum at 60 deg C for 12 h.

Scalability contextSmall 20 mg LSCF batch; no yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	LSCF NFs	20 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	methanol	2 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	DMF	1 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Linker	HATP.6HCl ligand	3.5 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Metal Source	Ni(CH3COO)2.4H2O	5 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Complete recipeSource: Main

Route 4: Solvothermal

2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Metal precursors20 mg LSCF NFs; 10 mg Ni(CH3COO)2.4H2O

Linker precursors7 mg HATP.6HCl

Solvents2 mL methanol; 1 mL DMF

Temperature70

Time3

Work-upSame as LSCF@Ni3(HITP)2-1: sonication/dispersal, 70 deg C water bath, centrifugation, washing with DMF and ethanol.

ActivationDried under vacuum at 60 deg C for 12 h.

Scalability contextSmall 20 mg LSCF batch; no yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	LSCF NFs	20 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	methanol	2 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	DMF	1 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Linker	HATP.6HCl	7 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Metal Source	Ni(CH3COO)2.4H2O	10 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Complete recipeSource: Main

Route 5: Solvothermal

2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Metal precursors20 mg LSCF NFs; 20 mg Ni(CH3COO)2.4H2O

Linker precursors14 mg HATP.6HCl

Solvents2 mL methanol; 1 mL DMF

Temperature70

Time3

Work-upSame route as LSCF@Ni3(HITP)2-1 with altered HATP and nickel acetate amounts.

ActivationDried under vacuum at 60 deg C for 12 h.

Scalability contextSmall 20 mg LSCF batch; no yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	LSCF NFs	20 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	methanol	2 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	DMF	1 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Linker	HATP.6HCl	14 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Metal Source	Ni(CH3COO)2.4H2O	20 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Complete recipeSource: Main

Route 6: Solvothermal

2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Metal precursors20 mg LSCF NFs; 40 mg Ni(CH3COO)2.4H2O

Linker precursors28 mg HATP.6HCl

Solvents2 mL methanol; 1 mL DMF

Temperature70

Time3

Work-upSame route as LSCF@Ni3(HITP)2-1 with altered HATP and nickel acetate amounts.

ActivationDried under vacuum at 60 deg C for 12 h.

Scalability contextSmall 20 mg LSCF batch; no yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	LSCF NFs	20 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	methanol	2 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Solvent	DMF	1 mL	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Linker	HATP.6HCl	28 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2
Metal Source	Ni(CH3COO)2.4H2O	40 mg	2 · 2.3 Preparation of LSCF@Ni3(HITP)2

Vague recipeSource: Main

Route 7: Unknown

3 · Results and discussion · Fig. 2a

Metal precursorsnot reported for standalone bare Ni3(HITP)2 control

Linker precursorsnot reported for standalone bare Ni3(HITP)2 control