Synthesis · Ultrathin 2D metal-organic framework nanosheet arrays to boost the overall efficiency of water splitting

6 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

97 · 2.4. Preparation of electrodes

Metal precursorsRuO2 active material

Solventsnot reported

AdditivesAcetylene black; PVDF

Atmospherenot reported

Temperature65

Time6

Substrate orientationnickel foam; orientation not reported

Work-upSlurry deposited onto NF and dried.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	RuO2	active material; loading active materials ~1.0 mg total	97 · 2.4. Preparation of electrodes
Additive	acetylene black	8:1:1 active:acetylene black:PVDF mass ratio	97 · 2.4. Preparation of electrodes
Additive	PVDF	8:1:1 active:acetylene black:PVDF mass ratio	97 · 2.4. Preparation of electrodes

Partial recipeSource: Main

Route 2: Drop Cast

97 · 2.4. Preparation of electrodes

Metal precursors20 wt% Pt/C active material

Solventsnot reported

AdditivesAcetylene black; PVDF

Atmospherenot reported

Temperature65

Time6

Substrate orientationnickel foam; orientation not reported

Work-upSlurry deposited onto NF and dried.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	20 wt% Pt/C	active material; loading active materials ~1.0 mg total · 20 wt% Pt/C	97 · 2.4. Preparation of electrodes
Additive	acetylene black	8:1:1 active:acetylene black:PVDF mass ratio	97 · 2.4. Preparation of electrodes
Additive	PVDF	8:1:1 active:acetylene black:PVDF mass ratio	97 · 2.4. Preparation of electrodes

Partial recipeSource: Main

Route 3: Solvothermal

97 · 2.4. Preparation of electrodes

Metal precursorsNickel nitrate hexahydrate; nickel foam substrate

Linker precursorsTCPP; BPY

SolventsOriginal solvothermal mixture; DMF, ethanol and deionized water used for washing

AdditivesAcetic acid in original mixture

Atmospherenot reported

Temperature100

Time72

Substrate orientationnickel foam added to solvothermal mixture; orientation not reported

Work-upFiltration followed by thorough washing with DMF, ethanol and deionized water.

Activationnot separately reported for supported electrode

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	nickel foam	appropriate amount	97 · 2.4. Preparation of electrodes
Metal Source	nickel nitrate hexahydrate	as in TIT-1 synthesis · 6 mol/L in DMF stock	97 · 2.4. Preparation of electrodes
Linker	TCPP	as in TIT-1 synthesis	97 · 2.4. Preparation of electrodes
Linker	BPY	as in TIT-1 synthesis	97 · 2.4. Preparation of electrodes

Partial recipeSource: Main

Route 4: Other

96 · 2.3. Synthesis of TIT-1@NS · Scheme 1

Metal precursorsTIT-1 precursor contains Ni nodes

Linker precursorsTIT-1 precursor contains TCPP and BPY

SolventsSolvent not named for ultrasonication; wash solvents were deionized water, ethanol and DMF

Atmospherenot reported

Temperatureambient/not reported

Time0.5 h ultrasonication/stirring; 24 h lyophilisation

Work-upMultiple wash cycles with deionized water, ethanol and DMF, followed by centrifugation.

ActivationLyophilization for 24 h.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	TIT-1	not reported	96 · 2.3. Synthesis of TIT-1@NS · Scheme 1
Solvent	deionized water	wash solvent	96 · 2.3. Synthesis of TIT-1@NS · Scheme 1
Solvent	ethanol	wash solvent	96 · 2.3. Synthesis of TIT-1@NS · Scheme 1
Solvent	dimethylformamide (DMF)	wash solvent	96 · 2.3. Synthesis of TIT-1@NS · Scheme 1

Partial recipeSource: Main

Route 5: Solvothermal

97 · 2.4. Preparation of electrodes

Metal precursorsNickel nitrate hexahydrate; nickel foam substrate

Linker precursorsTCPP; BPY

SolventsOriginal solvothermal mixture; DMF, ethanol and deionized water used for washing

AdditivesAcetic acid in original mixture

Atmospherenot reported

Temperature100

Time72

Substrate orientationnickel foam added to solvothermal mixture; orientation not reported

Work-upFiltration followed by thorough washing with DMF, ethanol and deionized water.

Activationnot separately reported for supported electrode

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	nickel foam	appropriate amount	97 · 2.4. Preparation of electrodes
Metal Source	nickel nitrate hexahydrate	as in TIT-1 synthesis · 6 mol/L in DMF stock	97 · 2.4. Preparation of electrodes
Linker	TCPP	as in TIT-1 synthesis	97 · 2.4. Preparation of electrodes
Linker	BPY	as in TIT-1 synthesis	97 · 2.4. Preparation of electrodes

Complete recipeSource: Main

Route 6: Solvothermal

96 · 2.2. Synthesis of TIT-1

Metal precursorsNickel nitrate hexahydrate, 1 drop of 6 mol/L DMF solution

Linker precursorsTCPP, 15 mg; BPY, 15 mg

SolventsDMA (2 mL); H2O (2 mL); DMF in nickel nitrate stock solution

AdditivesAcetic acid, 5 drops

Atmospherenot reported

Temperature100

Time72

Work-upWashed three times with ethanol.

ActivationDehydrated in a vacuum oven at 65 deg C for 12 h.

Show 6 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	nickel nitrate hexahydrate	1 drop · 6 mol/L in DMF	96 · 2.2. Synthesis of TIT-1
Linker	TCPP	15 mg	96 · 2.2. Synthesis of TIT-1
Linker	BPY	15 mg	96 · 2.2. Synthesis of TIT-1
Solvent	DMA	2 mL	96 · 2.2. Synthesis of TIT-1
Solvent	H2O	2 mL	96 · 2.2. Synthesis of TIT-1
Acid	acetic acid	5 drops	96 · 2.2. Synthesis of TIT-1