Synthesis evidence

Electrically Conductive Metal–Organic Framework Thin Film-Based On-Chip Micro-Biosensor: A Platform to Unravel Surface Morphology-Dependent Biosensing

Chen X., Dong J., Chi K. et al. · Advanced Functional Materials · 2021 · 2102855

5 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

p008 · Experimental Section - Transfer Method · Figure 1g

Solventsaqueous/organic reaction liquid during Langmuir-Schaefer-like transfer
Atmosphereambient
Substrate orientationsilicon wafer positioned horizontally to approach and contact the Cu-BHT film, giving bottom-side upward films
Work-upFilm adsorbed/transferred onto substrate; later processed into device if needed.
Complete recipeSource: Both

Route 2: Air Liquid Interface

p007 · Experimental Section - Preparation of Cu-BHT Films

Metal precursorsCu(NO3)2 aqueous solution, 50 mL, 1 mM
Linker precursorsbenzenehexathiol (BHT), 0.1 mM in chlorobenzene, 20 uL
Solventschlorobenzene organic phase; acidic aqueous solution
AdditivesHCl to pH = 1
Atmosphereair atmosphere; ambient surrounding environment
Temperatureambient temperature
Timefilm visible within 5 min; morphology tracked from 5 to 60 min; transferred after solvent evaporation
Substrate orientationfilm formed floating at aqueous/organic interface before transfer
Oxidant / reductantCu(II) nitrate precursor reduced during Cu-BHT formation; no added reductant specified
Work-upAfter organic solvent evaporated, the nearly transparent floating film was transferred onto hydrophilically treated substrates.
ActivationNo separate activation reported.
Scalability contextVery thin films (<20 nm) were obtained; six-film thickness and conductivity RSDs indicate reproducible preparation.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(NO3)250 mL · 1 mMp007 · Experimental Section - Preparation of Cu-BHT Films
Linkerbenzenehexathiol (BHT)0.1 mMp007 · Experimental Section - Preparation of Cu-BHT Films
Solventchlorobenzene20 uLp007 · Experimental Section - Preparation of Cu-BHT Films
AcidHClto pH = 1p007 · Experimental Section - Preparation of Cu-BHT Films
Complete recipeSource: Main

Route 3: Other

p008 · Experimental Section - Fabrication of the Cu-BHT Film-Based On-Chip Micro-Biosensor · Figure S12

Metal precursorsCr/Au electrode deposition, 5 nm Cr / 20 nm Au
Additivesphotoresists LOR3A and S1813; PDMS slot
Atmosphereoxygen plasma during electrode treatment and etching
Substrate orientation2 x 2 cm silicon wafer with 300 nm dielectric layer; Cu-BHT transferred by Langmuir-Schaefer method
Oxidant / reductantoxygen plasma etching removes excess Cu-BHT
Work-upSpin-coat photoresist, UV lithography, Cr/Au physical vapour deposition, oxygen plasma treatment, Cu-BHT transfer, second lithography/development, oxygen plasma etch, photoresist removal, PDMS slot installation.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherLOR3A photoresistNot specifiedp008 · Experimental Section - Fabrication of the Cu-BHT Film-Based On-Chip Micro-Biosensor · Figure S12
OtherS1813 photoresistNot specifiedp008 · Experimental Section - Fabrication of the Cu-BHT Film-Based On-Chip Micro-Biosensor · Figure S12
OtherCr/Au5 nm Cr / 20 nm Aup008 · Experimental Section - Fabrication of the Cu-BHT Film-Based On-Chip Micro-Biosensor · Figure S12
OtherPDMS slotNot specifiedp008 · Experimental Section - Fabrication of the Cu-BHT Film-Based On-Chip Micro-Biosensor · Figure S12
Complete recipeSource: Main

Route 4: Other

p008 · Experimental Section - Hydrophilic Treatment of the Substrate

SolventsDI water, ethanol, acetone
AdditivesPiranha solution H2SO4 (95-98%) / H2O2 (30%) = 2:1
Atmospherenitrogen purge after cleaning
Temperature80
Time2 h piranha treatment; 5 min each ultrasonic cleaning step; dried in oven
Substrate orientationSi/SiO2 substrates cleaned before film transfer
Oxidant / reductantH2O2 in piranha solution
Work-upRinsed and ultrasonically cleaned for 5 min with pure ethanol and acetone; nitrogen purged and dried at 80 deg C.
ActivationHydrophilic surface treatment only.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Solventdeionized waterNot specifiedp008 · Experimental Section - Hydrophilic Treatment of the Substrate
SolventethanolNot specifiedp008 · Experimental Section - Hydrophilic Treatment of the Substrate
SolventacetoneNot specifiedp008 · Experimental Section - Hydrophilic Treatment of the Substrate
OxidantH2SO4/H2O2 piranha solution2:1 · H2SO4 95-98%; H2O2 30%p008 · Experimental Section - Hydrophilic Treatment of the Substrate
Complete recipeSource: Main

Route 5: Other

p008 · Experimental Section - Transfer Method · Figure 1d

Solventsaqueous/organic reaction liquid during Langmuir-Schaefer-like transfer
Atmosphereambient
Substrate orientationsubstrate inserted obliquely under film and pulled vertically out of liquid to expose the up-side surface upward
Work-upFilm adsorbed/transferred onto substrate; later processed into device if needed.