Synthesis · Facile formation of a nanostructured NiP2@C material for advanced lithium-ion battery anode using adsorption property of metal-organic framework

4 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

2 · Supporting Information · Fig. S2

Metal precursorsas-synthesised Ni-MOF-74

Linker precursorsDOBDC-containing Ni-MOF-74 framework

ActivationActivated Ni-MOF-74 is named and its PXRD is shown/referenced, but activation conditions are not reported in the main text or SI text layer.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	as-synthesised Ni-MOF-74	Not specified	2 · Supporting Information · Fig. S2

Complete recipeSource: Main

Route 2: Solvothermal

2 · Synthesis of Ni-MOF-74

Metal precursorsNi(NO3)2.6H2O (119 mg, 0.41 mmol)

Linker precursorsH4DOBDC (0.478 g, 2.41 mmol; H4DOBDC = 2,5-dihydroxyterephthalic acid)

SolventsDMF-ethanol-water, 1:1:1 volume ratio, 10 mL

Atmospheresealed 25 mL reaction kettle; no inert atmosphere specified

Temperature100

Time72

Work-upultrasonicated for 30 min before heating; cooled to room temperature; product filtered

Scalability contextReaction in a 25 mL kettle with 10 mL solvent; product described as yellow microcrystalline material.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Ni(NO3)2.6H2O	119 mg, 0.41 mmol	2 · Synthesis of Ni-MOF-74
Linker	H4DOBDC (2,5-dihydroxyterephthalic acid)	0.478 g, 2.41 mmol	2 · Synthesis of Ni-MOF-74
Solvent	DMF-ethanol-water	10 mL, 1:1:1 volume ratio	2 · Synthesis of Ni-MOF-74

Partial recipeSource: Main

Route 3: Other

2 · Synthesis of nanostructured NiP2@C · Scheme 1

Metal precursorsactivated Ni-MOF-74 (0.5 g)

Linker precursorsNi-MOF-74 organic linkers, carbonised in situ to porous carbon

Additivesred phosphorus powder (0.5 g)

Atmosphereground in glove box; calcined under argon gas flow

Temperature600

Time2

Oxidant / reductantred phosphorus acts as phosphorus source

Work-upfurnace completely cooled to room temperature; product removed; colour changed from purple to black

Activationuses activated Ni-MOF-74; activation conditions not specified

Scalability contextUses 0.5 g activated Ni-MOF-74 and 0.5 g red phosphorus in a combustion boat/tube furnace.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	activated Ni-MOF-74	0.5 g	2 · Synthesis of nanostructured NiP2@C · Scheme 1
Additive	red phosphorus powders	0.5 g	2 · Synthesis of nanostructured NiP2@C · Scheme 1

Complete recipeSource: Main

Route 4: Drop Cast

2 · Electrochemical measurements

Metal precursorsNiP2@C nanocomposite

SolventsN-methyl-2-pyrrolidinone (NMP)

AdditivesSuper-P carbon black; polyvinylidene fluoride (PVDF); electrolyte 1 M LiPF6 in EC/DMC for cell assembly

AtmosphereAr-filled glove box with moisture and oxygen concentrations lower than 0.1 ppm for coin-cell assembly

Temperature100

Time24

Substrate orientationcopper foil current collector

Oxidant / reductantlithium metal counter/reference electrode

Work-upslurry pasted onto copper foil and dried in vacuum at 100 degrees C for 24 h; assembled as CR2032 coin-type half-cells

Scalability contextElectrode formulation uses 80:10:10 active material:conductive carbon:binder by weight.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	NiP2@C	80 wt% in electrode mixture	2 · Electrochemical measurements
Additive	Super-P carbon black	10 wt% in electrode mixture	2 · Electrochemical measurements
Additive	polyvinylidene fluoride (PVDF)	10 wt% in electrode mixture	2 · Electrochemical measurements
Solvent	N-methyl-2-pyrrolidinone (NMP)	Not specified	2 · Electrochemical measurements
Electrolyte	LiPF6 in ethylene carbonate/dimethyl carbonate	1 M LiPF6; EC:DMC = 1:1 by volume · 1 M	2 · Electrochemical measurements