Synthesis evidence

Thermally Driven Resistive Switching in Solution-Processable Thin Films of Coordination Polymers

Rana S., Prasoon A., Jha P.K. et al. · Journal of Physical Chemistry Letters · 2017 · 5008-5014

3 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Liquid Liquid Interface

S2 · Experimental Section · Growth of Ag-TCNQ Thin Film (step II)

Metal precursorsAgNO3 ethanolic solution
Linker precursorsTCNQ ethanolic solution
Solventsethanol
Additivespreformed Cu-TCNQ thin film grown on carboxy-terminated MUDA SAM/Au
Atmospheredrying atmosphere not explicitly specified for step II; N2 drying used for step I workup
Temperature60
Time0.5 h in AgNO3 solution plus 0.5 h in TCNQ solution per cycle; 10 cycles
Substrate orientationpreformed Cu-TCNQ thin film on MUDA SAM/Au-coated silicon substrate
Oxidant / reductantCu(I) in CuTCNQ proposed to reduce Ag(I) to Ag(0); Ag(0) then reacts with TCNQ to form AgTCNQ
Work-upSI does not explicitly state wash/dry workup for step II; main text describes repeated dipping in AgNO3 and TCNQ solutions.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceAgNO3not explicitly reported for step IIS2 · Experimental Section · Growth of Ag-TCNQ Thin Film (step II)
LinkerTCNQnot explicitly reported for step IIS2 · Experimental Section · Growth of Ag-TCNQ Thin Film (step II)
SolventethanolNot specifiedS2 · Experimental Section · Growth of Ag-TCNQ Thin Film (step II)
ReductantCu-TCNQ sacrificial thin filmNot specifiedS2 · Experimental Section · Growth of Ag-TCNQ Thin Film (step II)
Vague recipeSource: Main

Route 2: Unknown

5013 · Main text · Figure 6

Work-uppressed into pellet before transport and C-V measurements
Complete recipeSource: Both

Route 3: Liquid Liquid Interface

S2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)

Metal precursors1 mM Cu(OAc)2.H2O in ethanol
Linker precursors1 mM TCNQ in ethanol
Solventsethanol; ethanol/acetic acid (v:v = 9:1) for MUDA SAM preparation; piranha solution for Au-wafer cleaning
Additivesmercaptoundecanoic acid (MUDA) carboxy-terminated SAM on Au-coated silicon substrate
AtmosphereN2 gas stream used for drying after wafer cleaning, SAM preparation and each LbL step
Temperature60
Time0.5 h in metal ion solution plus 0.5 h in TCNQ solution per cycle; 10 cycles; SAM formation 48 h; piranha cleaning 0.5 h
Substrate orientationAu (100 nm) on silicon wafer bearing carboxy-terminated MUDA SAM
Work-upAfter each Cu(OAc)2.H2O or TCNQ dip, substrate was washed with ethanol and dried in a stream of N2 gas.
Scalability contextLayer-by-layer growth repeated for 10 cycles to grow thick thin films; the paper emphasises controllable thickness for LbL films but does not report batch scale.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2.H2O1 mMS2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)
LinkerTCNQ1 mMS2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)
SolventethanolNot specifiedS2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)
Additivemercaptoundecanoic acid (MUDA)1 mM for SAM preparationS2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)
Acidacetic acidethanol:acetic acid v:v = 9:1 for SAM preparationS2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)
OxidantH2O2 in piranha cleaning solutionH2SO4 (95%-98%)/H2O2 (30%) v/v 2:1S2 · Experimental Section · Growth of Cu-TCNQ Thin Film (step I)