Synthesis · Self-supporting electrochemical sensors for monitoring of cell-released H2O2 based on metal nanoparticle/MOF nanozymes

7 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Drop Cast

main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Metal precursorsAs-prepared 2D Zn-MOF nanosheets

SolventsUltrapure water with Nafion (5%), v:v = 1:0.010

AdditivesNafion 5%

Atmospheredried at room temperature; N2 used for cleaned GCE drying

Temperatureroom temperature

Timesonicated 10 min; drying time not specified

Substrate orientationglassy carbon electrode

Work-up10 uL homogeneous suspension dropped onto cleaned GCE and dried.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	2D Zn-MOF nanosheets	10 uL suspension · 1.0 mg mL-1	main p.3 · 2.2. Electrochemical preparation of sensing electrodes
Additive	Nafion (5%)	water:Nafion v:v = 1:0.010 · 5%	main p.3 · 2.2. Electrochemical preparation of sensing electrodes
Solvent	ultrapure water	Not specified	main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Complete recipeSource: SI

Route 2: Solvothermal

SI pp.S3-S4 · S1.3. Synthesis of 2D Zn-MOF nanosheets

Metal precursorsZn(NO3)2.6H2O, 4.5 mg, 0.015 mmol

Linker precursorsTCPP, 4.0 mg, 0.005 mmol; pyrazine, 0.8 mg, 0.01 mmol

SolventsDMF/ethanol, v:v = 3:1; 12 mL initial solvent plus 4 mL TCPP solution

AdditivesPVP, 20.0 mg

Atmospherenot specified

Temperature80

Time16

Substrate orientationnot_applicable

Work-upWashed consecutively with ethanol twice; after each washing centrifuged at 8000 rpm for 10 min.

ActivationVacuum dried at 65 C for 30 h.

Scalability context20 mL capped vial batch; no scale-up discussed.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(NO3)2.6H2O	4.5 mg, 0.015 mmol	SI pp.S3-S4 · S1.3. Synthesis of 2D Zn-MOF nanosheets
Linker	TCPP	4.0 mg, 0.005 mmol	SI pp.S3-S4 · S1.3. Synthesis of 2D Zn-MOF nanosheets
Linker	pyrazine	0.8 mg, 0.01 mmol	SI pp.S3-S4 · S1.3. Synthesis of 2D Zn-MOF nanosheets
Additive	PVP	20.0 mg	SI pp.S3-S4 · S1.3. Synthesis of 2D Zn-MOF nanosheets
Solvent	DMF and ethanol	12 mL plus 4 mL · V:V = 3:1	SI pp.S3-S4 · S1.3. Synthesis of 2D Zn-MOF nanosheets

Complete recipeSource: Main

Route 3: Drop Cast

main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Metal precursorsAs-prepared 3D Zn-MOF nanocrystals

SolventsUltrapure water with Nafion (5%), v:v = 1:0.010

AdditivesNafion 5%

Atmospheredried at room temperature; N2 used for cleaned GCE drying

Temperatureroom temperature

Timesonicated 10 min; drying time not specified

Substrate orientationglassy carbon electrode

Work-up10 uL homogeneous suspension dropped onto cleaned GCE and dried.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	3D Zn-MOF nanocrystals	10 uL suspension · 1.0 mg mL-1	main p.3 · 2.2. Electrochemical preparation of sensing electrodes
Additive	Nafion (5%)	water:Nafion v:v = 1:0.010 · 5%	main p.3 · 2.2. Electrochemical preparation of sensing electrodes
Solvent	ultrapure water	Not specified	main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Complete recipeSource: SI

Route 4: Other

SI p.S4 · S1.4. Fabrication of polyhedral 3D Zn-MOF nanocrystals

Metal precursorsZn(NO3)2.6H2O, 1.68 g in 20 mL methanol

Linker precursors2-methylimidazole, 4 g in 60 mL methanol

SolventsMethanol

Atmospherenot specified

Temperature25 reaction; 60 vacuum drying

Time1 h stirring plus 24 h incubation; dried overnight

Substrate orientationnot_applicable

Work-upCentrifuged at 6000 rpm for 10 min; washed several times with deionized water and MeOH.

ActivationDried at 60 C overnight under vacuum.

Scalability contextReported product mass 1.06 g and conversion yield 84.5%.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	Zn(NO3)2.6H2O	1.68 g · in 20 mL methanol	SI p.S4 · S1.4. Fabrication of polyhedral 3D Zn-MOF nanocrystals
Linker	2-methylimidazole	4 g · in 60 mL methanol	SI p.S4 · S1.4. Fabrication of polyhedral 3D Zn-MOF nanocrystals
Solvent	methanol	80 mL total	SI p.S4 · S1.4. Fabrication of polyhedral 3D Zn-MOF nanocrystals

Complete recipeSource: Main

Route 5: Electrochemical

main pp.3,5 · 2.2 and 3.1 · Fig. 1

Metal precursorsAgNO3, 1.0 mM

Linker precursors2D Zn-MOF/GCE support

Solventsaqueous electrodeposition solution, solvent not otherwise specified

AtmosphereN2 drying after washing

Temperatureroom temperature

Time150 s electrodeposition selected as optimum for Ag

Substrate orientation2D Zn-MOF modified glassy carbon electrode

Oxidant / reductantPotentiostatic reduction/deposition at -0.2 V vs Ag/AgCl

Work-upWashed thoroughly with ultrapure water and dried by N2.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	AgNO3	1.0 mM	main pp.3,5 · 2.2 and 3.1 · Fig. 1
Other	2D Zn-MOF/GCE	Not specified	main pp.3,5 · 2.2 and 3.1 · Fig. 1

Complete recipeSource: Main

Route 6: Electrochemical

main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Metal precursorsAgNO3, 1.0 mM

Linker precursors3D Zn-MOF/GCE support

Solventsaqueous electrodeposition solution, solvent not otherwise specified

AtmosphereN2 drying after washing

Temperatureroom temperature

Time150 s electrodeposition inferred from Ag optimum

Substrate orientation3D Zn-MOF modified glassy carbon electrode

Oxidant / reductantPotentiostatic reduction/deposition at -0.2 V vs Ag/AgCl

Work-upWashed thoroughly with ultrapure water and dried by N2.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	AgNO3	1.0 mM	main p.3 · 2.2. Electrochemical preparation of sensing electrodes
Other	3D Zn-MOF/GCE	Not specified	main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Complete recipeSource: Main

Route 7: Electrochemical

main p.3 · 2.2. Electrochemical preparation of sensing electrodes

Metal precursorsAgNO3, 1.0 mM

Solventsaqueous electrodeposition solution, solvent not otherwise specified

AtmosphereN2 drying after washing

Temperatureroom temperature

Time150 s optimum

Substrate orientationbare GCE

Oxidant / reductantPotentiostatic deposition at -0.2 V vs Ag/AgCl

Work-upWashed with ultrapure water and dried by N2.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Metal Source	AgNO3	1.0 mM	main p.3 · 2.2. Electrochemical preparation of sensing electrodes