Synthesis evidence

Electrically regulating nonlinear optical limiting of metal-organic framework film

Ma Z.-Z., Li Q.-H., Wang Z. et al. · Nature Communications · 2022 · 6347

4 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1

Metal precursorsCu(OAc)2*2H2O (1 mM)
Linker precursorsHHTP (0.015 mM)
Solventsethanol
Atmospherenot specified
Temperature40
Time0.4167 per cycle plus washing; 10 cycles total
Substrate orientationfunctionalized ITO glass; [001]-oriented film
Work-upBetween each metal/linker step, washed with ethanol to remove residual reactants.
Activationnot specified after film growth
Scalability context10 in situ LPE LBL growth cycles; film area not reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2*2H2O1 mM7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
LinkerHHTP0.015 mM7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
SolventethanolNot specified7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
Complete recipeSource: Main

Route 2: Other

7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1

Metal precursorsCu(OAc)2*2H2O (2 mM)
Linker precursorsHHTP (0.02 mM)
Solventsdeionized water
Additives10 uL NMP added to 100 mL HHTP solution
Atmospherenot specified
Temperature70
Time0.4167 per cycle plus washing; 15 cycles total
Substrate orientationfunctionalized ITO glass; [100]-oriented film
Work-upBetween each metal/linker step, washed with deionized water to remove residual reactants.
Activationnot specified after film growth
Scalability context15 in situ LPE LBL growth cycles; film area not reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2*2H2O2 mM7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
LinkerHHTP0.02 mM7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
Solventdeionized waterNot specified7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
AdditiveNMP10 uL added to 100 mL HHTP solution7 · Fabrication of Cu-HHTP films with different orientations · Fig. 1
Complete recipeSource: Main

Route 3: Solvothermal

7 · Fabrication of Cu-HHTP Powder

Metal precursorsCu(OAc)2*2H2O (10 mg)
Linker precursors2,3,6,7,10,11-hexahydroxytriphenylene (HHTP, 7 mg)
Solventsdeionized water (4 mL); 1-methyl-2-pyrrolidone (NMP, 0.165 mL)
AdditivesNMP added dropwise
Atmospherenot specified; capped vial
Temperature85
Time36
Work-upNatural cooling to room temperature; centrifugation; washed three times with deionized water and acetone.
ActivationDried under vacuum.
Scalability context20 mL vial batch; no scale-up reported.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker2,3,6,7,10,11-hexahydroxytriphenylene (HHTP)7 mg7 · Fabrication of Cu-HHTP Powder
Metal SourceCu(OAc)2*2H2O10 mg7 · Fabrication of Cu-HHTP Powder
Solventdeionized water4 mL7 · Fabrication of Cu-HHTP Powder
Additive1-methyl-2-pyrrolidone (NMP)0.165 mL7 · Fabrication of Cu-HHTP Powder
Complete recipeSource: Main

Route 4: Other

7 · Preparation of functionalized substrates

Solventsdeionized water, ethanol, acetone
Additivesconcentrated H2O2 (30%) and NaOH (2 mmol) aqueous solution, volume ratio 1:3
Atmospheredried under nitrogen flux
Temperature80
Time0.5
Substrate orientationITO glass substrate functionalization
Oxidant / reductantH2O2
Work-upSequential ultrasonication in deionized water, ethanol and acetone; treated with H2O2/NaOH; cleaned with deionized water.
ActivationDried under nitrogen flux.
Scalability contextSubstrate pretreatment; no batch area reported.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Solventdeionized water, ethanol, acetoneNot specified7 · Preparation of functionalized substrates
Oxidantconcentrated hydrogen peroxide30%7 · Preparation of functionalized substrates
BaseNaOH aqueous solution2 mmol7 · Preparation of functionalized substrates