Synthesis · Enhancing electrochemical hydrogen storage in nickel-based metal-organic frameworks (MOFs) through zinc and cobalt doping as bimetallic MOFs

8 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Solvothermal

349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Metal precursorsCoCl2 and Ni(NO3)2.6H2O at 8:34:58 CoCl2:Ni(NO3)2.6H2O:TPA weight ratio

Linker precursorsterephthalic acid (TPA)

SolventsDMF (20 mL); DMF and alcohol for washing

Additives2 mL 0.4 M NaOH solution

Atmospherenot specified

Temperature100

Time8

Work-upNatural cooling; precipitate collected and washed several times with DMF and alcohol

ActivationDried at 120 C for 12 h under ambient conditions

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CoCl2	weight ratio component 8	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Metal Source	Ni(NO3)2.6H2O	weight ratio component 34	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Linker	terephthalic acid (TPA)	weight ratio component 58	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Solvent	DMF	20 mL	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Base	NaOH solution	2 mL · 0.4 M	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Partial recipeSource: Main

Route 2: Solvothermal

349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Metal precursorsCoCl2 and Ni(NO3)2.6H2O at 15:31:54 CoCl2:Ni(NO3)2.6H2O:TPA weight ratio

Linker precursorsterephthalic acid (TPA)

SolventsDMF (20 mL); DMF and alcohol for washing

Additives2 mL 0.4 M NaOH solution

Atmospherenot specified

Temperature100

Time8

Work-upNatural cooling; precipitate collected and washed several times with DMF and alcohol

ActivationDried at 120 C for 12 h under ambient conditions

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CoCl2	weight ratio component 15	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Metal Source	Ni(NO3)2.6H2O	weight ratio component 31	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Linker	terephthalic acid (TPA)	weight ratio component 54	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Solvent	DMF	20 mL	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Base	NaOH solution	2 mL · 0.4 M	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Partial recipeSource: Main

Route 3: Solvothermal

349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Metal precursorsCoCl2 and Ni(NO3)2.6H2O at 26:27:47 CoCl2:Ni(NO3)2.6H2O:TPA weight ratio

Linker precursorsterephthalic acid (TPA)

SolventsDMF (20 mL); DMF and alcohol for washing

Additives2 mL 0.4 M NaOH solution

Atmospherenot specified

Temperature100

Time8

Work-upNatural cooling; precipitate collected and washed several times with DMF and alcohol

ActivationDried at 120 C for 12 h under ambient conditions

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CoCl2	weight ratio component 26	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Metal Source	Ni(NO3)2.6H2O	weight ratio component 27	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Linker	terephthalic acid (TPA)	weight ratio component 47	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Solvent	DMF	20 mL	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Base	NaOH solution	2 mL · 0.4 M	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Complete recipeSource: Main

Route 4: Solvothermal

349 · 2.2. Preparation of pure Ni(TPA) MOF

Metal precursorsNiCl2.6H2O (0.21 g, 0.88 mmol)

Linker precursorsterephthalic acid (TPA; 0.16 g, 0.96 mmol)

SolventsDMF (20 mL); ethanol and DI water for washing

Atmospherenot specified

Temperature120

Time24

Work-upNatural cooling to room temperature; washed three times with ethanol and DI water

ActivationDried overnight at 100 C under vacuum

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Linker	terephthalic acid (TPA)	0.16 g, 0.96 mmol	349 · 2.2. Preparation of pure Ni(TPA) MOF
Metal Source	NiCl2.6H2O	0.21 g, 0.88 mmol	349 · 2.2. Preparation of pure Ni(TPA) MOF
Solvent	DMF	20 mL	349 · 2.2. Preparation of pure Ni(TPA) MOF
Solvent	ethanol	wash solvent	349 · 2.2. Preparation of pure Ni(TPA) MOF
Solvent	DI water	wash solvent	349 · 2.2. Preparation of pure Ni(TPA) MOF

Partial recipeSource: Main

Route 5: Drop Cast

349 · 2.3.1. Electrochemical measurement

Metal precursorssynthesized MOF

Solventspure ethanol; THF and DI water for Cu foam cleaning

Atmosphereambient

Temperature60

Time2

Substrate orientationporous copper foam, 1 cm2

Work-upCu foam cleaned with THF and DI water and dried at 60 C for 2 h; MOF dispersion drop-cast onto Cu foam

ActivationDried at 60 C for 2 h after drop-casting

Scalability contextElectrode fabrication by drop-casting; exact ethanol volume and coating-area details beyond 1 cm2 not specified.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	synthesized MOF	0.1 mg material utilized for working electrode	349 · 2.3.1. Electrochemical measurement
Solvent	ethanol	dispersion solvent	349 · 2.3.1. Electrochemical measurement
Other	porous copper foam	1 cm2	349 · 2.3.1. Electrochemical measurement
Solvent	THF	cleaning solvent	349 · 2.3.1. Electrochemical measurement
Solvent	DI water	cleaning solvent	349 · 2.3.1. Electrochemical measurement

Partial recipeSource: Main

Route 6: Solvothermal

349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Metal precursorsZnCl2 and Ni(NO3)2.6H2O at 8:34:58 ZnCl2:Ni(NO3)2.6H2O:TPA weight ratio

Linker precursorsterephthalic acid (TPA)

SolventsDMF (20 mL); DMF and alcohol for washing

Additives2 mL 0.4 M NaOH solution

Atmospherenot specified

Temperature100

Time8

Work-upNatural cooling; precipitate collected and washed several times with DMF and alcohol

ActivationDried at 120 C for 12 h under ambient conditions

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZnCl2	weight ratio component 8	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Metal Source	Ni(NO3)2.6H2O	weight ratio component 34	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Linker	terephthalic acid (TPA)	weight ratio component 58	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Solvent	DMF	20 mL	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Base	NaOH solution	2 mL · 0.4 M	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Partial recipeSource: Main

Route 7: Solvothermal

349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Metal precursorsZnCl2 and Ni(NO3)2.6H2O at 15:31:54 ZnCl2:Ni(NO3)2.6H2O:TPA weight ratio

Linker precursorsterephthalic acid (TPA)

SolventsDMF (20 mL); DMF and alcohol for washing

Additives2 mL 0.4 M NaOH solution

Atmospherenot specified

Temperature100

Time8

Work-upNatural cooling; precipitate collected and washed several times with DMF and alcohol

ActivationDried at 120 C for 12 h under ambient conditions

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZnCl2	weight ratio component 15	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Metal Source	Ni(NO3)2.6H2O	weight ratio component 31	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Linker	terephthalic acid (TPA)	weight ratio component 54	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Solvent	DMF	20 mL	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Base	NaOH solution	2 mL · 0.4 M	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Partial recipeSource: Main

Route 8: Solvothermal

349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs

Metal precursorsZnCl2 and Ni(NO3)2.6H2O at 26:27:47 ZnCl2:Ni(NO3)2.6H2O:TPA weight ratio

Linker precursorsterephthalic acid (TPA)

SolventsDMF (20 mL); DMF and alcohol for washing

Additives2 mL 0.4 M NaOH solution

Atmospherenot specified

Temperature100

Time8

Work-upNatural cooling; precipitate collected and washed several times with DMF and alcohol

ActivationDried at 120 C for 12 h under ambient conditions

Scalability context40 mL Teflon-lined stainless-steel autoclave batch.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	ZnCl2	weight ratio component 26	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Metal Source	Ni(NO3)2.6H2O	weight ratio component 27	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Linker	terephthalic acid (TPA)	weight ratio component 47	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Solvent	DMF	20 mL	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs
Base	NaOH solution	2 mL · 0.4 M	349 · 2.3. Preparation of Zn- and Co-doped Ni(TPA) MOFs