Synthesis evidence

Processable UiO-66 Metal-Organic Framework Fluid Gel and Electrical Conductivity of Its Nanofilm with Sub-100 nm Thickness

Somjit V., Thinsoongnoen P., Waiprasoet S. et al. · ACS Applied Materials and Interfaces · 2021 · 30844-30852

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: Solvothermal

p002 / 30845 · Synthesis of UiO-66 Fluid Gel

Metal precursorsZrOCl2.8H2O, same as UiO-66 procedure
Linker precursorsfumaric acid (0.56 g, 4.83 mmol)
SolventsDMF; DI water; ethanol, same as UiO-66 procedure
Additives37 wt% HCl and glacial acetic acid, same as UiO-66 procedure
AtmosphereStatic conditions; atmosphere not otherwise specified
Temperature100
Time2
Work-upSame washing, centrifugation, DI water dispersion, sonication, and ethanol storage method as UiO-66 fluid gel.
ActivationNot separately specified for synthesis; adsorption activation not reported for MOF-801.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrOCl2.8H2Osame as UiO-66 procedurep002 / 30845 · Synthesis of UiO-66 Fluid Gel
Linkerfumaric acid0.56 g, 4.83 mmolp002 / 30845 · Synthesis of UiO-66 Fluid Gel
SolventDMFsame as UiO-66 procedurep002 / 30845 · Synthesis of UiO-66 Fluid Gel
Acid37 wt % HClsame as UiO-66 procedure · 37 wt %p002 / 30845 · Synthesis of UiO-66 Fluid Gel
Acidglacial acetic acidsame as UiO-66 procedurep002 / 30845 · Synthesis of UiO-66 Fluid Gel
Partial recipeSource: Main

Route 2: Other

p005 / 30848 · Results and Discussion · Figure 4c

Metal precursorsMOF-801 fluid gel
SolventsDI water dispersion
Atmospherenot specified
Temperature100
Time20.1667
Substrate orientationcleaned glass substrates
Work-upMOF-801 fluid gel spun on cleaned glass substrates using the same method/optimal spin-coating parameters from UiO-66.
ActivationSame annealing procedure as UiO-66 films.
Scalability contextSpecific concentration/spin speed for MOF-801 was not stated; authors say optimal UiO-66 parameters were applied.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMOF-801 fluid gelNot specifiedp005 / 30848 · Results and Discussion · Figure 4c
Solventdeionized waterNot specifiedp005 / 30848 · Results and Discussion · Figure 4c
Otherglass substrateNot specifiedp005 / 30848 · Results and Discussion · Figure 4c
Complete recipeSource: Main

Route 3: Solvothermal

p002 / 30845 · Synthesis of UiO-66 Fluid Gel

Metal precursorsZrOCl2.8H2O, same as UiO-66 procedure
Linker precursorstrimesic acid (1.01 g, 4.83 mmol)
SolventsDMF; DI water; ethanol, same as UiO-66 procedure
Additives37 wt% HCl and glacial acetic acid, same as UiO-66 procedure
AtmosphereStatic conditions; atmosphere not otherwise specified
Temperature100
Time2
Work-upSame washing, centrifugation, DI water dispersion, sonication, and ethanol storage method as UiO-66 fluid gel.
ActivationNot separately specified for synthesis; adsorption activation not reported for MOF-808.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrOCl2.8H2Osame as UiO-66 procedurep002 / 30845 · Synthesis of UiO-66 Fluid Gel
Linkertrimesic acid1.01 g, 4.83 mmolp002 / 30845 · Synthesis of UiO-66 Fluid Gel
SolventDMFsame as UiO-66 procedurep002 / 30845 · Synthesis of UiO-66 Fluid Gel
Acid37 wt % HClsame as UiO-66 procedure · 37 wt %p002 / 30845 · Synthesis of UiO-66 Fluid Gel
Acidglacial acetic acidsame as UiO-66 procedurep002 / 30845 · Synthesis of UiO-66 Fluid Gel
Partial recipeSource: Main

Route 4: Other

p005 / 30848 · Results and Discussion · Figure 4d

Metal precursorsMOF-808 fluid gel
SolventsDI water dispersion
Atmospherenot specified
Temperature100
Time20.1667
Substrate orientationcleaned glass substrates
Work-upMOF-808 fluid gel spun on cleaned glass substrates using the same method/optimal spin-coating parameters from UiO-66.
ActivationSame annealing procedure as UiO-66 films.
Scalability contextSpecific concentration/spin speed for MOF-808 was not stated; authors say optimal UiO-66 parameters were applied.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherMOF-808 fluid gelNot specifiedp005 / 30848 · Results and Discussion · Figure 4d
Solventdeionized waterNot specifiedp005 / 30848 · Results and Discussion · Figure 4d
Otherglass substrateNot specifiedp005 / 30848 · Results and Discussion · Figure 4d
Complete recipeSource: Main

Route 5: Other

p002 / 30845 · Fabrication of UiO-66 Thin-Film Device for Electrical Measurement · Figure 5a,b

Metal precursorsUiO-66 fluid gel; Al electrode metal
SolventsDI water dispersion for spin-cast fluid gel
Atmosphereglovebox under inert N2 atmosphere for test device fabrication
Temperature100
Time20.1667
Substrate orientationcleaned glass substrate, 2.5 x 2.5 cm2
Work-up40 nm Al anode thermally evaporated through a shadow mask; UiO-66 fluid gel spin-cast and annealed; 40 nm Al cathode thermally evaporated.
ActivationAl deposition pressure below 5 x 10^-6 Pa at 1.0 A s^-1; device area 0.04 cm2.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherAl40 nm anode and 40 nm cathodep002 / 30845 · Fabrication of UiO-66 Thin-Film Device for Electrical Measurement · Figure 5a,b
OtherUiO-66 fluid gelNot specifiedp002 / 30845 · Fabrication of UiO-66 Thin-Film Device for Electrical Measurement · Figure 5a,b
Othercleaned glass substrate2.5 x 2.5 cm2p002 / 30845 · Fabrication of UiO-66 Thin-Film Device for Electrical Measurement · Figure 5a,b
Complete recipeSource: Main

Route 6: Solvothermal

p002 / 30845 · Synthesis of UiO-66 Fluid Gel

Metal precursorsZrOCl2.8H2O (1.07 g, 3.33 mmol)
Linker precursorsterephthalic acid (0.80 g, 4.83 mmol)
SolventsDMF (20 mL); DI water dispersion; ethanol storage
Additives37 wt% HCl (0.5 mL); glacial acetic acid (0.67 mL)
AtmosphereStatic conditions in sealed 50 mL Duran bottle; atmosphere not otherwise specified
Temperature100
Time2
Work-upWashed thrice with DMF (20 mL) and thrice with ethanol (20 mL) using 5 C precooling centrifugation at 12,500 rpm for 30 min; 0.10 g product dispersed in DI water (1 mL) and sonicated 1 h at room temperature.
ActivationKept in ethanol at room temperature for further use; adsorption samples degassed at 150 C under vacuum for 24 h before adsorption measurements.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZrOCl2.8H2O1.07 g, 3.33 mmolp002 / 30845 · Synthesis of UiO-66 Fluid Gel
Linkerterephthalic acid0.80 g, 4.83 mmolp002 / 30845 · Synthesis of UiO-66 Fluid Gel
SolventDMF20 mLp002 / 30845 · Synthesis of UiO-66 Fluid Gel
Acid37 wt % HCl0.5 mL · 37 wt %p002 / 30845 · Synthesis of UiO-66 Fluid Gel
Acidglacial acetic acid0.67 mLp002 / 30845 · Synthesis of UiO-66 Fluid Gel
Solventdeionized water1 mLp002 / 30845 · Synthesis of UiO-66 Fluid Gel
Solventethanol20 mL x 3 washes; storage solventp002 / 30845 · Synthesis of UiO-66 Fluid Gel
Complete recipeSource: Main

Route 7: Other

p002 / 30845 · Fabrication of UiO-66 Thin Film by Spin-Coating · Figure 4; Figure S4

Metal precursorsUiO-66 fluid gel
SolventsDI water dispersion
AtmosphereAmbient during spin coating not specified; vacuum oven used for final drying
Temperature100
Time20.1667
Substrate orientationcleaned glass substrates
Work-upGlass substrates cleaned by sonication in liquid detergent, DI water, acetone, and isopropanol for 10 min each; UV-ozone 20 min. UiO-66 fluid gel dispensed statically and spun at 1000-5000 rpm for 60 s.
ActivationAnnealed on hot plate at 100 C for 10 min and in vacuum oven at 100 C for 20 h.
Scalability contextFilm thickness was tuned by fluid-gel concentration and spin speed; full coverage occurred above 0.100 g mL^-1.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
OtherUiO-66 fluid gel0.025 to 0.500 g mL^-1 studiedp002 / 30845 · Fabrication of UiO-66 Thin Film by Spin-Coating · Figure 4; Figure S4
Solventdeionized waterNot specifiedp002 / 30845 · Fabrication of UiO-66 Thin Film by Spin-Coating · Figure 4; Figure S4
Otherglass substrateNot specifiedp002 / 30845 · Fabrication of UiO-66 Thin Film by Spin-Coating · Figure 4; Figure S4