Synthesis · NiCo-MOFs in situ anchored on graphdiyne with metal-like properties form a strongly coupled electron transport interface and construct an ohmic contact to achieve efficient charge-hole spatial separation

4 structured synthesis routes

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

Vague recipeSource: Main

Route 1: Other

2 · Preparation of Cu-GDY (CG)

Metal precursorscopper sulfate reduced to elemental Cu powder

Linker precursorsgraphdiyne precursor not fully specified in text; Fig. 1 indicates an alkyne coupling route

Solventsdeionized water for Cu reduction; graphdiyne-coupling solvent not fully specified in text

Additivesascorbic acid reducing agent; pyridine mentioned as dissolving/precipitating Cu+ during alkyne coupling

Atmospherenitrogen protection during Cu powder drying

Substrate orientationCu powder used instead of copper foil

Oxidant / reductantascorbic acid

Work-upCu powder dried under nitrogen; further CG workup not reported in main text

Scalability contextPowder route intended to avoid copper-foil purification before photocatalytic suspension use.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	copper sulfate	not reported	2 · Preparation of Cu-GDY (CG)
Reductant	ascorbic acid	not reported	2 · Preparation of Cu-GDY (CG)
Solvent	deionized water	not reported	2 · Preparation of Cu-GDY (CG)
Additive	pyridine	not reported	2 · Preparation of Cu-GDY (CG)

Partial recipeSource: Main

Route 2: Solvothermal

2 · Preparation of the NiCo-MOF (NC) and the composite catalyst

Metal precursorsnickel nitrate and cobalt nitrate

Linker precursors1,3,5-trimesic acid

SolventsN,N-dimethylformamide

Atmospherenot specified

Temperature170

Time16

Work-upwashed with alcohol several times and dried in a vacuum oven at 70 C

Activationvacuum drying at 70 C

Scalability contextBatch solvothermal route in a 50 mL reactor; exact metal/linker masses for NC are not reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel nitrate	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Metal Source	cobalt nitrate	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Linker	1,3,5-trimesic acid	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Solvent	N,N-dimethylformamide	30 mL inferred from analogous NCCG-15 route	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst

Partial recipeSource: Main

Route 3: Solvothermal

2 · Preparation of the NiCo-MOF (NC) and the composite catalyst

Metal precursorsnickel nitrate and cobalt nitrate

Linker precursors1,3,5-trimesic acid

Solvents30 mL N,N-dimethylformamide

Additives10 mg CG

Atmospherenot specified

Temperature170

Time16

Substrate orientationin situ growth on dispersed CG

Work-upwashed with alcohol several times and dried in a vacuum oven at 70 C

Activationvacuum drying at 70 C

Scalability context50 mL reactor, 30 mL DMF; no yield reported.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	CG	10 mg	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Solvent	N,N-dimethylformamide	30 mL	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Metal Source	nickel nitrate	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Metal Source	cobalt nitrate	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Linker	1,3,5-trimesic acid	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst

Partial recipeSource: Main

Route 4: Solvothermal

2 · Preparation of the NiCo-MOF (NC) and the composite catalyst

Metal precursorsnickel nitrate and cobalt nitrate

Linker precursors1,3,5-trimesic acid

SolventsN,N-dimethylformamide

AdditivesCG amount varied to obtain X = 5, 10, 20, and 25

Atmospherenot specified

Temperature170

Time16

Substrate orientationin situ growth on dispersed CG

Work-upwashed with alcohol several times and dried in a vacuum oven at 70 C

Activationvacuum drying at 70 C

Scalability contextVariant preparation changes only CG amount according to the main text.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Additive	CG	varied; exact masses not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Solvent	N,N-dimethylformamide	not individually reported for variants	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Metal Source	nickel nitrate	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Metal Source	cobalt nitrate	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst
Linker	1,3,5-trimesic acid	not reported	2 · Preparation of the NiCo-MOF (NC) and the composite catalyst