cMOF Evidence Base

Synthesis evidence

Large-Area Synthesis of Ultrathin, Flexible, and Transparent Conductive Metal–Organic Framework Thin Films via a Microfluidic-Based Solution Shearing Process

Lee T., Kim J.-O., Park C. et al. · Advanced Materials · 2022 · 2107696

4 structured synthesis routes

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

Partial recipeSource: SI

Route 1: Drop Cast

9 · Chemiresistive gas sensing measurement

Metal precursorsbulk Ni3(HITP)2 powder, synthesis recipe not described
Solventsethanol dispersion
Atmospheredrying atmosphere not specified
Temperature60 deg C drying
Substrate orientationdrop-coated on interdigitated sensor substrate three times
Work-up3 mg powder in 150 uL ethanol; 5 uL suspension drop-coated three times and dried at 60 deg C.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
OtherNi3(HITP)2 powder3 mg9 · Chemiresistive gas sensing measurement
Solventethanol150 uL9 · Chemiresistive gas sensing measurement
Partial recipeSource: Both

Route 2: Solution Shearing

8 · Synthesis of Co3(HITP)2 thin-film using MASS-PRC process · Figure S10

Metal precursorsCo(NO3)2.6H2O, 37.26 mM in DMF, 5-25 uL/min
Linker precursorsHATP.6HCl, 19.73 mM in DMF, 5-25 uL/min
SolventsDMF
AdditivesTEA, 2 wt% in DMF, 90 deg C
Atmospherenot specified
Temperatureheated substrate during ejection; TEA 90 deg C
TimeTEA treatment 10 min
Substrate orientationmicrofluidic channel, ejected at 10-50 uL/min; other parameters apparently same as MASS-PRC process
Work-upPost-TEA wash/dry not specified for Co3(HITP)2.
Scalability contextPresented as evidence that MASS-PRC is applicable to other conductive MOFs.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCo(No3)2.6H2O37.26 mM in DMF, 5-25 uL/min8 · Synthesis of Co3(HITP)2 thin-film using MASS-PRC process · Figure S10
LinkerHATP.6HCl19.73 mM in DMF, 5-25 uL/min8 · Synthesis of Co3(HITP)2 thin-film using MASS-PRC process · Figure S10
SolventDMFNot specified8 · Synthesis of Co3(HITP)2 thin-film using MASS-PRC process · Figure S10
BaseTEA2 wt% in DMF · 90 deg C, 10 min8 · Synthesis of Co3(HITP)2 thin-film using MASS-PRC process · Figure S10
Complete recipeSource: Both

Route 3: Solution Shearing

7 · Synthesis of Ni3(HITP)2 thin-film using MASS-PRC process

Metal precursorsNiCl2.6H2O, 29.87 mM in DMF, 5-25 uL/min
Linker precursorsHATP.6HCl, 19.73 mM in DMF, 5-25 uL/min
SolventsDMF for precursor streams; ethanol wash
AdditivesTEA, 2 wt% in DMF, 90 deg C post-treatment
AtmosphereN2 gas blow-dry after ethanol wash; other atmosphere not specified
Temperatureheated substrate during ejection; TEA post-treatment 90 deg C; substrate functionalisation 80-90 deg C where applicable
TimeTEA post-treatment 10 min; substrate cleaning 30 min; APTMS 30 min; HMDA 24 h for PI
Substrate orientationshearing speed 0.02-0.10 mm/s; blade angle 30 deg; 100 um blade-substrate gap; substrate heated
Work-upAfter solvent evaporation, soak in TEA solution; wash finished film with ethanol and blow with N2 gas.
ActivationFor BET sample only: scraped films evacuated at p < 1e-5 mbar at 393 K for 5 h.
Scalability contextLarge-area films over >50 x 70 mm; processing time <30 min; continuous microfluidic supply maintains solution volume and concentration.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O29.87 mM in DMF, 5-25 uL/min7 · Synthesis of Ni3(HITP)2 thin-film using MASS-PRC process
LinkerHATP.6HCl19.73 mM in DMF, 5-25 uL/min7 · Synthesis of Ni3(HITP)2 thin-film using MASS-PRC process
SolventN,N-dimethylformamide (DMF)Not specified7 · Synthesis of Ni3(HITP)2 thin-film using MASS-PRC process
Basetriethylamine (TEA)2 wt% in DMF · 90 deg C, 10 min7 · Synthesis of Ni3(HITP)2 thin-film using MASS-PRC process
AdditiveAPTMS or HMDA substrate functionalisation reagentsAPTMS 1 wt% in ethanol; HMDA 10 v/v% in DI water7 · Synthesis of Ni3(HITP)2 thin-film using MASS-PRC process
Partial recipeSource: SI

Route 4: Solution Shearing

8 · Synthesis of Ni3(HITP)2@Pt thin-film · Figure S21

Metal precursorsNiCl2.6H2O and PtCl2, 29.87 mM and 1.88 mM respectively in DMF
Linker precursorsHATP.6HCl solution
SolventsDMF
AdditivesTEA post-treatment as in bare Ni3(HITP)2 route
Atmospherenot specified
Temperaturesame as bare Ni3(HITP)2 thin-film fabrication
Timesame as bare Ni3(HITP)2 thin-film fabrication
Substrate orientationsame as bare Ni3(HITP)2 thin-film fabrication
Work-upsame as bare Ni3(HITP)2 thin-film fabrication
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O29.87 mM in DMF8 · Synthesis of Ni3(HITP)2@Pt thin-film · Figure S21
AdditivePtCl21.88 mM in DMF8 · Synthesis of Ni3(HITP)2@Pt thin-film · Figure S21
LinkerHATP.6HCl solutionNot specified8 · Synthesis of Ni3(HITP)2@Pt thin-film · Figure S21
SolventDMFNot specified8 · Synthesis of Ni3(HITP)2@Pt thin-film · Figure S21