Synthesis · Dual single atomic Fe-Ni sites in N‑doped nanoporous carbon for high-efficiency potassium periodate activation toward pollutant abatement

11 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

2 · 2.1.4 Synthesis of FeNi-NC, M-NC, and NC

Metal precursorsM-ZnO/ZIF-8 or ZnO/ZIF-8 hybrid powders

Linker precursorsZIF-8-derived organic linker carbon/nitrogen source

AtmosphereN2

Temperature900

Time2

Work-upPrepared using the same pyrolysis procedure as FeNi-NC.

ActivationThermal carbonisation/activation at 900 deg C.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	M-ZnO/ZIF-8 (M = Fe, Ni) or ZnO/ZIF-8 hybrid	not restated for each control	2 · 2.1.4 Synthesis of FeNi-NC, M-NC, and NC
Other	nitrogen	tube furnace atmosphere	2 · 2.1.4 Synthesis of FeNi-NC, M-NC, and NC

Complete recipeSource: Both

Route 2: Other

2 · 2.1.4 Synthesis of FeNi-NC, M-NC, and NC · Figure 1a

Metal precursorsFe&Ni-ZnO/ZIF-8 powder, 500 mg

Linker precursorsZIF-8-derived organic linker carbon/nitrogen source

AtmosphereN2

Temperature900

Time2

Work-upCalcined in tube furnace; no post-calcination acid washing is reported in the main text.

ActivationThermal carbonisation/activation at 900 deg C.

Scalability context500 mg precursor batch reported for calcination.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Fe&Ni-ZnO/ZIF-8 powder	500 mg	2 · 2.1.4 Synthesis of FeNi-NC, M-NC, and NC · Figure 1a
Other	nitrogen	tube furnace atmosphere	2 · 2.1.4 Synthesis of FeNi-NC, M-NC, and NC · Figure 1a

Complete recipeSource: Both

Route 3: Other

2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles

Metal precursorsZn(CH3COO)2.2H2O, 1.008 g; Fe(CH3COO)2, 0.0403 g

SolventsDMSO, 46 mL; ethanol solution of tetramethylammonium hydroxide; ethyl acetate, 110 mL; ethanol redispersion, 6 mL

Additivestetramethylammonium hydroxide pentahydrate, 0.1 g/mL in ethanol, 14 mL

Work-upBase solution added dropwise at about 2 mL/min; ethyl acetate added; Fe-ZnO nanoparticles centrifugally separated and redispersed in ethanol.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(CH3COO)2.2H2O	1.008 g	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Metal Source	Fe(CH3COO)2	0.0403 g	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Solvent	dimethyl sulfoxide (DMSO)	46 mL	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Base	tetramethylammonium hydroxide pentahydrate in ethanol	14 mL solution · 0.1 g/mL	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Solvent	ethyl acetate	110 mL	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Solvent	ethanol	6 mL redispersion	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles

Complete recipeSource: Both

Route 4: Other

2 · 2.1.3

Metal precursorsFe-ZnO solution, 800 uL; ZnO solution, 400 uL

Linker precursorsZIF-8, 1.20 g

Solventsethanol, 120 mL

Time14 h stirring after ultrasonication

Work-upSame assembly procedure as Fe&Ni-ZnO/ZIF-8; product obtained by centrifugal drying.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	ZIF-8	1.20 g	2 · 2.1.3
Metal Source	Fe-ZnO ethanol solution	800 uL · 25 mg/mL	2 · 2.1.3
Metal Source	ZnO ethanol solution	400 uL · 25 mg/mL	2 · 2.1.3
Solvent	ethanol	120 mL	2 · 2.1.3

Partial recipeSource: Both

Route 5: Other

2-3 · 2.1.3 · Figure 1a

Metal precursorsFe-ZnO and Ni-ZnO nanoparticle ethanol solutions; exact Fe&Ni-ZnO mixture volumes for Fe2Ni1 not fully specified in text

Linker precursorsZIF-8, 1.20 g

Solventsethanol, 120 mL

Time14 h stirring after ultrasonication

Work-upZIF-8 sonicated 5 min in ethanol; Fe&Ni-ZnO NPs added; additional 5 min ultrasonication; stirred 14 h; precursor obtained by centrifugal drying.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	ZIF-8	1.20 g	2-3 · 2.1.3 · Figure 1a
Solvent	ethanol	120 mL	2-3 · 2.1.3 · Figure 1a
Metal Source	Fe&Ni-ZnO nanoparticle ethanol mixture	not explicitly stated in main text for Fe2Ni1 precursor	2-3 · 2.1.3 · Figure 1a

Complete recipeSource: Both

Route 6: Other

2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles

Metal precursorsZn(CH3COO)2.2H2O, 1.008 g; Ni(CH3COO)2.4H2O, 56 mg

SolventsDMSO; ethanol; ethyl acetate

Additivestetramethylammonium hydroxide pentahydrate ethanol solution

Work-upPrepared by the same method as Fe-ZnO nanoparticles and redispersed as a 20 mg/mL ethanol solution.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(CH3COO)2.2H2O	1.008 g, inferred from identical Fe-ZnO protocol	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Metal Source	Ni(CH3COO)2.4H2O	56 mg	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Solvent	DMSO / ethanol / ethyl acetate	as Fe-ZnO protocol	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Base	tetramethylammonium hydroxide pentahydrate	as Fe-ZnO protocol · 0.1 g/mL in ethanol	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles

Complete recipeSource: Both

Route 7: Other

2 · 2.1.3

Metal precursorsZnO solution, 800 uL; Ni-ZnO solution, 400 uL

Linker precursorsZIF-8, 1.20 g

Solventsethanol, 120 mL

Time14 h stirring after ultrasonication

Work-upSame assembly procedure as Fe&Ni-ZnO/ZIF-8; product obtained by centrifugal drying.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	ZIF-8	1.20 g	2 · 2.1.3
Metal Source	ZnO ethanol solution	800 uL · 25 mg/mL	2 · 2.1.3
Metal Source	Ni-ZnO ethanol solution	400 uL · 20 mg/mL	2 · 2.1.3
Solvent	ethanol	120 mL	2 · 2.1.3

Complete recipeSource: Both

Route 8: Other

8 · 3.4 Durability and practical application · Figure 4e

Metal precursorsused Fe2Ni1-NC-900

AtmosphereN2

Temperature900

Time2

Work-upUsed catalyst annealed after recycling deactivation.

ActivationAnnealing treatment to remove adsorption products and restore defect level.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	used Fe2Ni1-NC-900	Not specified	8 · 3.4 Durability and practical application · Figure 4e
Other	nitrogen	annealing atmosphere	8 · 3.4 Durability and practical application · Figure 4e

Complete recipeSource: Both

Route 9: Solvothermal

2 · 2.1.1 Preparation of ZIF-8

Metal precursorsZn(NO3)2.6H2O, 3.348 g

Linker precursors2-methylimidazole, 3.696 g

Solventsmethanol, 90 mL

Temperature120

Time2

Work-upNatural cooling; white precipitates gathered; washed multiple times with ethanol; dried overnight.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(NO3)2.6H2O	3.348 g	2 · 2.1.1 Preparation of ZIF-8
Linker	2-methylimidazole	3.696 g	2 · 2.1.1 Preparation of ZIF-8
Solvent	methanol	90 mL	2 · 2.1.1 Preparation of ZIF-8
Solvent	ethanol	multiple washes	2 · 2.1.1 Preparation of ZIF-8

Complete recipeSource: Both

Route 10: Other

2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles

Metal precursorsZn(CH3COO)2.2H2O, 1.008 g

SolventsDMSO; ethanol; ethyl acetate

Additivestetramethylammonium hydroxide pentahydrate ethanol solution

Work-upPrepared by the same protocol as Fe-ZnO nanoparticles, omitting iron acetate; redispersed at 25 mg/mL.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(CH3COO)2.2H2O	1.008 g, inferred from identical Fe-ZnO protocol	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Solvent	DMSO / ethanol / ethyl acetate	as Fe-ZnO protocol	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles
Base	tetramethylammonium hydroxide pentahydrate	as Fe-ZnO protocol · 0.1 g/mL in ethanol	2 · 2.1.2 Preparation of ZnO and M-ZnO nanoparticles

Complete recipeSource: Both

Route 11: Other

2 · 2.1.3

Metal precursorspure ZnO ethanol solution, 1200 uL

Linker precursorsZIF-8, 1.20 g

Solventsethanol, 120 mL

Time14 h stirring after ultrasonication

Work-upSame assembly procedure as Fe&Ni-ZnO/ZIF-8; product obtained by centrifugal drying.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	ZIF-8	1.20 g	2 · 2.1.3
Metal Source	ZnO ethanol solution	1200 uL · 25 mg/mL	2 · 2.1.3
Solvent	ethanol	120 mL	2 · 2.1.3