cMOF Evidence Base

Synthesis evidence

Large-area synthesis of nanoscopic catalyst-decorated conductive MOF film using microfluidic-based solution shearing

Kim J.-O., Koo W.-T., Kim H. et al. · Nature Communications · 2021 · 4294

5 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Solution Shearing

6 · Methods

Metal precursorscopper(II) acetate monohydrate, 0.12 M in DMSO, 200 uL/min
Linker precursorsHHTP, 0.1 M in DMSO, 200 uL/min
SolventsDMSO; ethanol and DMSO washes
Atmosphereair not otherwise specified; substrates oxygen-plasma-treated before coating
Temperature150
Timecontinuous flow; Supplementary Table 1 reports 10 min process time
Substrate orientationblade-substrate gap 100 um; blade angle 30 deg; glass, silicon wafer, or Al2O3 substrates
Work-upwashed with DMSO and ethanol
Activationfor BET samples, evacuated at P < 1e-5 mbar at 393 K for 5 h
Scalability context64 outlets, 15-cycle serpentine mixing, large-area solution shearing; described as high-throughput up to 5 mm/s.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper(II) acetate monohydrate0.12 M in DMSO6 · Methods
LinkerHHTP0.1 M in DMSO6 · Methods
SolventDMSONot specified6 · Methods
Partial recipeSource: Main

Route 2: Drop Cast

7 · Methods

Metal precursorspre-existing Cu3(HHTP)2 powder; powder synthesis not reported
Solventsethanol
Atmosphereair
Temperatureroom temperature sensing; drop-cast drying not specified
Substrate orientationAl2O3 substrate, 2.5 mm x 2.5 mm x 0.2 mm; Au electrodes with 70 um gap
Work-upsensor stabilised by fresh air for 4 h before NO2 tests
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Solventethanol300 uL7 · Methods
OtherCu3(HHTP)2 powder5 mg7 · Methods
Vague recipeSource: Main

Route 3: Solution Shearing

3 · Results · Fig. 2f

Metal precursorsall Pt@Cu3(HHTP)2 components premixed as bulk solution; exact concentrations for comparison route not restated
Linker precursorsall components premixed as bulk solution
SolventsDMSO inferred from main MiCS recipe
AdditivesNaBH4 inferred from Pt@Cu3(HHTP)2 chemistry
Atmosphereair not specified
Temperature150
Substrate orientationbulk solution inserted between blade and substrate before coating
Oxidant / reductantNaBH4 likely present; not separately specified for conventional comparison
Scalability contextUsed as lower-uniformity comparison, not the optimised route.
Complete recipeSource: Both

Route 4: Solution Shearing

5 · Sensing characteristics · Supplementary Fig. 16 and Supplementary Table 6

Metal precursorsas route_pt_cu3_hhtp2_mics_thinfilm, with Pt precursor solution varied at 50, 100, 150, and 200 uL/min
Linker precursorsHHTP, 0.1 M in DMSO, mixed with NaBH4 at 1 mg/mL
SolventsDMSO; ethanol and DMSO washes
AdditivesNaBH4, 1 mg/mL
Atmosphereair not otherwise specified
Temperature150
Timecontinuous flow; process time not separately stated for each loading
Substrate orientationPt solution inserted at 9th cycle; 100 um gap; 30 deg angle
Oxidant / reductantNaBH4 reduction of Pt precursor
Work-upwashed with DMSO and ethanol
Scalability contextPt flow-rate series used for sensor optimisation.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Metal Sourcepotassium tetrachloroplatinate(II) (K2PtCl4)50, 100, 150, or 200 uL/min · 1 mg/mL5 · Sensing characteristics · Supplementary Fig. 16 and Supplementary Table 6
Complete recipeSource: Both

Route 5: Solution Shearing

7 · Methods

Metal precursorscopper(II) acetate monohydrate, 0.12 M in DMSO, 200 uL/min; potassium tetrachloroplatinate(II) Pt precursor solution, 1 mg/mL, 100 uL/min for optimised 2.3 wt% Pt sample
Linker precursorsHHTP, 0.1 M in DMSO, mixed with NaBH4 at 1 mg/mL, 200 uL/min
SolventsDMSO; ethanol and DMSO washes
AdditivesNaBH4, 1 mg/mL
Atmosphereair not otherwise specified; substrates oxygen-plasma-treated before coating
Temperature150
Timecontinuous flow; Supplementary Table 1 reports 10 min process time
Substrate orientationPt solution inserted at 9th mixing cycle; blade-substrate gap 100 um; blade angle 30 deg
Oxidant / reductantNaBH4 reduces Pt precursor; also present during Cu3(HHTP)2 nucleation
Work-upwashed with DMSO and ethanol
Activationfor BET samples, evacuated at P < 1e-5 mbar at 393 K for 5 h
Scalability contextMiCS simultaneously synthesises Pt@Cu3(HHTP)2 particles and grows large-area film during solution shearing.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal Sourcecopper(II) acetate monohydrate0.12 M in DMSO7 · Methods
Metal Sourcepotassium tetrachloroplatinate(II) (K2PtCl4)Pt solution flow 100 uL/min for optimised sample · 1 mg/mL7 · Methods
LinkerHHTP0.1 M in DMSO7 · Methods
Reductantsodium borohydride (NaBH4)1 mg/mL7 · Methods
SolventDMSONot specified7 · Methods