Synthesis · Spindle-like Ni3(HITP)2 MOFs: Synthesis and Li+ storage mechanism

Complete recipeSource: Main

Route 1: Drop Cast

2 · 2.3 Electrochemical characterization

Metal precursorsNi3(HITP)2 powder active material

Solventsdeionized water; EC-DMC electrolyte during cell assembly

Additivesconductive carbon; CMC/SBR binder; 1 M LiPF6 electrolyte; Celgard 2300 separator

Atmosphereargon glove box for coin-cell assembly; O2 and H2O below 0.1 ppm

Temperature100 drying; 25 electrochemical tests

Time10 h drying

Substrate orientationcopper foil current collector

Oxidant / reductantlithium counter electrode in LIR 2016 coin cell

Work-upSlurry spread on copper foil by blade, dried under vacuum, cut into a round plate.

ActivationElectrochemical cycling in Li half-cell.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni3(HITP)2 powder	60 wt% in electrode slurry	2 · 2.3 Electrochemical characterization
Additive	conductive carbon	20 wt% in electrode slurry	2 · 2.3 Electrochemical characterization
Additive	CMC/SBR binder mixture	20 wt% in electrode slurry; CMC:SBR = 1:1 by weight	2 · 2.3 Electrochemical characterization
Electrolyte	LiPF6 in EC-DMC	dropped into the cell · 1 M; EC-DMC 1:1 v:v	2 · 2.3 Electrochemical characterization

Complete recipeSource: Main

2 · 2.1 Synthesis of Ni3(HITP)2 MOFs

Metal precursorsnickel chloride hexahydrate (NiCl2.6H2O), 356.5 mg, 1.5 mmol, analytical grade

Linker precursors2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl), 0.5 mmol, 98%

Solventsdeionized water; ethanol wash

Additives14 mol L-1 NH4OH, 5 mmol, 10 times of HATP

Atmosphereair during ligand addition; drying under vacuum

Temperature65 reaction; 100 vacuum drying

Time2 h reaction at 65 C; 12 h water immersion; repeated immersion/filtration two more times; 12 h vacuum drying

Work-upCool to room temperature; filtration; immerse black powder in water for 12 h; repeat filtration/immersion two more times; wash with ethanol.

ActivationDried under vacuum at 100 C for 12 h to remove ethanol.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel chloride (NiCl2.6H2O)	356.5 mg, 1.5 mmol	2 · 2.1 Synthesis of Ni3(HITP)2 MOFs
Linker	2,3,6,7,10,11-hexaaminotriphenylene hexahydrochloride (HATP.6HCl)	0.5 mmol	2 · 2.1 Synthesis of Ni3(HITP)2 MOFs
Solvent	deionized water	50 ml for NiCl2 solution; 50 ml for HATP.6HCl solution	2 · 2.1 Synthesis of Ni3(HITP)2 MOFs
Base	NH4OH	5 mmol, 10 times of HATP · 14 mol L-1	2 · 2.1 Synthesis of Ni3(HITP)2 MOFs
Solvent	ethanol	washed with ethanol	2 · 2.1 Synthesis of Ni3(HITP)2 MOFs