Synthesis · High-Entropy Metal-Organic Framework Arrays Boost Oxygen Evolution Electrocatalysis

4 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Solvothermal

S2 · Synthesis of comparison MOF samples · Figures S4-S11

Metal precursorssingle-, double-, triple- and quadruple-metal subsets of the HE-MOF acetylacetonate metal sources

Linker precursors2,6-naphthalenedicarboxylate ligand

SolventsDI water and ethanol, inferred from same HE-MOF route

Atmospherenot specified

Temperature120

Time20

Substrate orientationnickel foam substrate, inferred from electrode comparisons and SEM captions

Work-upsame as HE-MOF route; details not separately stated

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel/cobalt/iron/zinc/molybdenum acetylacetonate subset	not separately stated for each comparison MOF	S2 · Synthesis of comparison MOF samples · Figures S4-S11
Linker	2,6-naphthalenedicarboxylate ligand	same way as HE-MOF; exact amount for comparison samples not separately stated	S2 · Synthesis of comparison MOF samples · Figures S4-S11

Complete recipeSource: Main

Route 2: Solvothermal

14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a

Metal precursors0.05 mmol each nickel acetylacetone, cobalt acetylacetone, iron acetylacetone, zinc acetylacetone and molybdenum acetylacetone

Linker precursors0.25 mmol organic ligand, described as 2,6-naphthalenedicarboxylate tetrahydrate; materials list gives 2,6-naphthalenedicarboxylic acid dipotassium salt

SolventsDI water and ethanol; 10 mL organic ligand solution added

Atmospherenot specified

Temperature120

Time20

Substrate orientationnickel foam present during solvothermal growth

Work-upcool to room temperature; wash with DI water three times

Scalability contextOne-step mild solvothermal synthesis on NF; no scale-up yield reported.

Show 9 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel acetylacetone	0.05 mmol	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Metal Source	cobalt acetylacetone	0.05 mmol	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Metal Source	iron acetylacetone	0.05 mmol	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Metal Source	zinc acetylacetone	0.05 mmol	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Metal Source	molybdenum acetylacetone	0.05 mmol	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Linker	organic ligand (2,6-naphthalenedicarboxylate tetrahydrate)	0.25 mmol; 10 mL of organic ligand solution	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Solvent	DI-water	mixture with EtOH · 18 Mohm cm-1 resistivity	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Solvent	EtOH, absolute	mixture with DI-water	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a
Other	nickel foam	NF substrate	14096 · 2.2. Synthesis of the HE-MOF Electrocatalyst · Figure 1a

Partial recipeSource: SI

Route 3: Drop Cast

S2 · Synthesis of HE-MOF bulk

Metal precursorsHE-MOF bulk material synthesised in the same way as HE-MOF but without NF

Linker precursors2,6-naphthalenedicarboxylate ligand, inferred from same synthesis

Solventsisopropanol/water (v/v = 1/3)

Additives1 wt% Nafion binder

Atmospherenot specified

Substrate orientationdrop-cast onto NF substrate

Work-updisperse HE-MOF powder in binder solution and drop-cast

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	HE-MOF powder	loading 0.76 mg cm-2	S2 · Synthesis of HE-MOF bulk
Additive	Nafion	1 wt%	S2 · Synthesis of HE-MOF bulk
Solvent	isopropanol/water	v/v = 1/3	S2 · Synthesis of HE-MOF bulk

Partial recipeSource: SI

Route 4: Other

S2 · Synthesis of HE-MOF powder

Metal precursorsHE-MOF array material

Atmospherenot specified

Work-upultrasonication exfoliation

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	HE-MOF	Not specified	S2 · Synthesis of HE-MOF powder