Synthesis · Tuning Lewis acidity of MIL-88B-Fe with mix-valence coordinatively unsaturated iron centers on ultrathin Ti3C2 nanosheets for efficient photo-Fenton reaction

7 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Hydrothermal

p.3 · Fig. S4

Metal precursorsTi3C2 nanosheets (0.2 g, from SI sample label); FeCl3.6H2O and MIL-88B-Fe precursors inferred from main route

Linker precursors1,4-benzenedicarboxylic acid, inferred from main composite route

SolventsDMF, inferred from main composite route

AdditivesTi3C2 nanosheets 0.2 g

AtmosphereNot specified in SI loading caption; main route uses vacuum for final activation

Temperature120 hydrothermal; 205 activation inferred from main route

Time12 hydrothermal; 12 activation inferred from main route

Oxidant / reductantThermal activation generates FeII/FeIII CUCs; no chemical reductant added.

Work-upNot repeated in SI; main route reports centrifugation and washing with water/DMF.

ActivationVacuum activation inferred from CUCs-MIL-88B-Fe/Ti3C2 label and main route.

Scalability contextOnly loading label is reported in SI figure; no scale-up data.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ti3C2 nanosheets	0.2 g	p.3 · Fig. S4
Metal Source	FeCl3.6H2O	not repeated in SI · not repeated in SI	p.3 · Fig. S4
Linker	1,4-benzenedicarboxylic acid	not repeated in SI · not repeated in SI	p.3 · Fig. S4
Solvent	DMF	not repeated in SI	p.3 · Fig. S4

Partial recipeSource: SI

Route 2: Hydrothermal

p.3 · Fig. S4

Metal precursorsTi3C2 nanosheets (0.3 g, from SI sample label); FeCl3.6H2O and MIL-88B-Fe precursors inferred from main route

Linker precursors1,4-benzenedicarboxylic acid, inferred from main composite route

SolventsDMF, inferred from main composite route

AdditivesTi3C2 nanosheets 0.3 g

AtmosphereNot specified in SI loading caption; main route uses vacuum for final activation

Temperature120 hydrothermal; 205 activation inferred from main route

Time12 hydrothermal; 12 activation inferred from main route

Oxidant / reductantThermal activation generates FeII/FeIII CUCs; no chemical reductant added.

Work-upNot repeated in SI; main route reports centrifugation and washing with water/DMF.

ActivationVacuum activation inferred from CUCs-MIL-88B-Fe/Ti3C2 label and main route.

Scalability contextOnly loading label is reported in SI figure; no scale-up data.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ti3C2 nanosheets	0.3 g	p.3 · Fig. S4
Metal Source	FeCl3.6H2O	not repeated in SI · not repeated in SI	p.3 · Fig. S4
Linker	1,4-benzenedicarboxylic acid	not repeated in SI · not repeated in SI	p.3 · Fig. S4
Solvent	DMF	not repeated in SI	p.3 · Fig. S4

Complete recipeSource: Main

Route 3: Other

p.2 · 2.2.2. Synthesis of CUCs-MIL-88B-Fe

Metal precursorsAs-prepared MIL-88B-Fe powder

Linker precursorsBDC already present in MIL-88B-Fe

AtmosphereVacuum

Temperature205

Time12

Oxidant / reductantThermal removal of coordinated guests/terminal species; no chemical reductant added.

Work-upStored in a small covered glass after activation.

Activation205 C under vacuum for 12 h.

Scalability contextCeramic boat/vacuum activation; no scale stated.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Other	as prepared MIL-88B-Fe powder	not reported	p.2 · 2.2.2. Synthesis of CUCs-MIL-88B-Fe

Complete recipeSource: Main

Route 4: Hydrothermal

p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2

Metal precursorsFeCl3.6H2O (1 mM; 0.270 mg, raw text); Ti3C2 nanosheets (100 mg)

Linker precursors1,4-benzenedicarboxylic acid (1 mM; 0.166 mg, raw text)

Solvents30 mL DMF

AdditivesTi3C2 nanosheets

AtmosphereNot specified for hydrothermal step; vacuum for activation

Temperature120 hydrothermal; 205 activation

Time12 hydrothermal; 12 activation

Oxidant / reductantThermal activation generates FeII/FeIII CUCs; no chemical reductant added.

Work-upCooled; isolated by centrifugation; washed with water and DMF several times.

ActivationAs-prepared MIL-88B-Fe/Ti3C2 powder activated at 205 C under vacuum for 12 h.

Scalability context100 mL Teflon-lined autoclave and ceramic boat/vacuum activation.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ti3C2 nanosheets	100 mg	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2
Metal Source	FeCl3.6H2O	0.270 mg · 1 mM	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2
Linker	1,4-benzenedicarboxylic acid	0.166 mg · 1 mM	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2
Solvent	DMF	30 mL	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2

Complete recipeSource: Main

Route 5: Hydrothermal

p.2 · 2.2.1. Synthesis of MIL-88B-Fe

Metal precursorsFeCl3.6H2O (1 mM; 0.270 mg, raw text)

Linker precursors1,4-benzenedicarboxylic acid (1 mM; 0.166 mg, raw text)

Solvents30 mL DMF

AtmosphereNot specified

Temperature120

Time12

Work-upCooled; isolated by centrifugation; washed with water and DMF several times.

ActivationNone reported for pristine MIL-88B-Fe.

Scalability context100 mL Teflon-lined autoclave batch; no scale-up data.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	FeCl3.6H2O	0.270 mg · 1 mM	p.2 · 2.2.1. Synthesis of MIL-88B-Fe
Linker	1,4-benzenedicarboxylic acid	0.166 mg · 1 mM	p.2 · 2.2.1. Synthesis of MIL-88B-Fe
Solvent	DMF	30 mL	p.2 · 2.2.1. Synthesis of MIL-88B-Fe

Complete recipeSource: Main

Route 6: Hydrothermal

p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2

Metal precursorsFeCl3.6H2O (1 mM; 0.270 mg, raw text); Ti3C2 nanosheets (100 mg)

Linker precursors1,4-benzenedicarboxylic acid (1 mM; 0.166 mg, raw text)

Solvents30 mL DMF

AdditivesTi3C2 nanosheets

AtmosphereNot specified for hydrothermal step

Temperature120

Time12

Work-upCooled; catalyst isolated by centrifugation; washed with water and DMF several times.

ActivationNone for intermediate sample.

Scalability context100 mL Teflon-lined autoclave batch.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ti3C2 nanosheets	100 mg	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2
Metal Source	FeCl3.6H2O	0.270 mg · 1 mM	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2
Linker	1,4-benzenedicarboxylic acid	0.166 mg · 1 mM	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2
Solvent	DMF	30 mL	p.2 · 2.2.4. Synthesis of CUCs-MIL-88B-Fe/Ti3C2

Complete recipeSource: Main

Route 7: Other

p.2 · 2.2.3. Synthesis of Ti3C2 nanosheets

Metal precursorsTi3AlC2 (2 g for etch; 1 g etched powder for intercalation)

Solvents49 wt% HF solution; DMSO; deionized water

AdditivesDMSO intercalant

AtmosphereNitrogen during DMSO intercalation and water exfoliation; not specified during HF etch/drying.

Temperature60 for HF etch; room temperature for intercalation/exfoliation

Time24 h HF etch; 18 h DMSO intercalation; 24 h ultrasonication

Oxidant / reductantHF selectively etches Al layer from Ti3AlC2.

Work-upCentrifuged, rinsed many times with deionized water, oven dried; after DMSO intercalation collected by centrifugation and washed with deionized water.

ActivationWater ultrasonication under N2 to exfoliate into few-layer MXene nanosheets.

Scalability contextGram-scale precursor amounts reported.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Ti3AlC2	2 g	p.2 · 2.2.3. Synthesis of Ti3C2 nanosheets
Acid	hydrogen fluoride solution	30 mL · 49 wt%	p.2 · 2.2.3. Synthesis of Ti3C2 nanosheets
Solvent	dimethyl sulfoxide (DMSO)	30 mL	p.2 · 2.2.3. Synthesis of Ti3C2 nanosheets
Solvent	deionized water	not reported	p.2 · 2.2.3. Synthesis of Ti3C2 nanosheets