Synthesis · Synthesis, structure, and lithium storage performance of non-conductive metal–organic frameworks for high-performance lithium-ion batteries

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries

Metal precursorsNi-mba-K active material

Solvents2-pyrrolidone / NMP

Additivesacetylene black; polyvinylidene fluoride (PVDF)

Atmosphereargon glove box for cell assembly

Temperature90

Time12

Substrate orientationcopper sheet current collector

Work-upgrind and disperse slurry; coat copper; dry at 90 deg C for 12 h; cut 12 mm circular sheet; assemble CR2032 button battery

Activationoven drying at 90 deg C for 12 h

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-mba-K active material	70 wt%	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Additive	acetylene black	10 wt%	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Additive	polyvinylidene fluoride (PVDF)	20 wt%	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Solvent	2-pyrrolidone (NMP)	Not specified	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Electrolyte	LiPF6 in EC:DMC:DEC	1 M; EC:DMC:DEC 1:1:1 w/w/w · 1 M	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries

Complete recipeSource: Main

Route 2: Solvothermal

2 · 2.3. Synthesis of Ni MOFs

Metal precursorsnickel chloride hexahydrate (NiCl2.6H2O, 3 mmol)

Linker precursors2-mercaptobenzoic acid / H2mba / mba (6 mmol)

Solventsanhydrous ethanol (20 mL); water in 10 mL aqueous nickel chloride solution

Additivespotassium hydroxide, equimolar replacement for NaOH (3 mmol inferred from NaOH recipe)

Atmospherenot reported; sealed Teflon-lined stainless-steel reactor

Temperature120

Time96

Work-upsame workup as Ni-mba-Na is implied: cool to 25 deg C; wash with deionized water, anhydrous ethanol, and dilute hydrochloric acid; dry at 90 deg C for 12 h

Activationdrying at 90 deg C for 12 h

Scalability contextyield about 23 wt% based on NiCl2.6H2O, H2mba and potassium hydroxide

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Base	potassium hydroxide	equimolar to NaOH; 3 mmol inferred	2 · 2.3. Synthesis of Ni MOFs
Linker	mba / H2mba / 2-mercaptobenzoic acid	6 mmol · dissolved with base in 20 mL anhydrous ethanol	2 · 2.3. Synthesis of Ni MOFs
Solvent	anhydrous ethanol	20 mL	2 · 2.3. Synthesis of Ni MOFs
Metal Source	nickel chloride hexahydrate	3 mmol · in 10 mL aqueous solution	2 · 2.3. Synthesis of Ni MOFs
Acid	dilute hydrochloric acid	used in wash by analogy to Ni-mba-Na route	2 · 2.3. Synthesis of Ni MOFs

Complete recipeSource: Main

Route 3: Other

2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries

Metal precursorsNi-mba-Na active material

Solvents2-pyrrolidone / NMP

Additivesacetylene black; polyvinylidene fluoride (PVDF)

Atmosphereargon glove box for cell assembly

Temperature90

Time12

Substrate orientationcopper sheet current collector

Work-upgrind and disperse slurry; coat copper; dry at 90 deg C for 12 h; cut 12 mm circular sheet; assemble CR2032 button battery

Activationoven drying at 90 deg C for 12 h

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ni-mba-Na active material	70 wt%	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Additive	acetylene black	10 wt%	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Additive	polyvinylidene fluoride (PVDF)	20 wt%	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Solvent	2-pyrrolidone (NMP)	Not specified	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries
Electrolyte	LiPF6 in EC:DMC:DEC	1 M; EC:DMC:DEC 1:1:1 w/w/w · 1 M	2 · 2.5. Preparation, assembly, and electrochemical measurements of electrode materials for lithium-ion batteries

Complete recipeSource: Main

Route 4: Solvothermal

2 · 2.3. Synthesis of Ni MOFs

Metal precursorsnickel chloride hexahydrate (NiCl2.6H2O, 3 mmol)

Linker precursors2-mercaptobenzoic acid / H2mba / mba (6 mmol)

Solventsanhydrous ethanol (20 mL); water in 10 mL aqueous nickel chloride solution

Additivessodium hydroxide (3 mmol)

Atmospherenot reported; sealed Teflon-lined stainless-steel reactor

Temperature120

Time96

Work-upcool to 25 deg C; wash several times with deionized water, anhydrous ethanol, and dilute hydrochloric acid; dry at 90 deg C for 12 h

Activationdrying at 90 deg C for 12 h

Scalability contextyield about 18 wt% based on NiCl2.6H2O, H2mba and sodium hydroxide

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Base	sodium hydroxide	3 mmol	2 · 2.3. Synthesis of Ni MOFs
Linker	mba / H2mba / 2-mercaptobenzoic acid	6 mmol · dissolved with NaOH in 20 mL anhydrous ethanol	2 · 2.3. Synthesis of Ni MOFs
Solvent	anhydrous ethanol	20 mL	2 · 2.3. Synthesis of Ni MOFs
Metal Source	nickel chloride hexahydrate	3 mmol · in 10 mL aqueous solution	2 · 2.3. Synthesis of Ni MOFs
Acid	dilute hydrochloric acid	used in wash	2 · 2.3. Synthesis of Ni MOFs