Synthesis evidence

Improved electrical conductivity of Co(ii) and Cu(ii) ladder polymers in the fabrication of photoresponsive Schottky devices

Dutta B., Das D., Raksha K. et al. · Materials Advances · 2022 · 215-222

4 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Other

218 · Device fabrication method · Scheme 1

Metal precursorspre-synthesised Co-CP
Linker precursorsnot applicable after CP synthesis
Solventsacetone, 2-propanol and distilled water used for ITO cleaning; coating dispersion solvent not reported
Additivesaluminium top contact
Atmospherevacuum oven drying; Al deposition at 4.7 x 10^-6 torr
Temperaturenot reported
Time1 h vacuum drying
Substrate orientationITO-coated glass substrate
Oxidant / reductantnone reported
Work-upspin-coated film dried in vacuum oven, then Al deposited through quad punch-hole shadow mask
Activationvacuum oven for 1 h
Scalability contextDevice area controlled by shadow mask; spin speed, film thickness and light intensity not reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
OtherITO-coated glass substratenot reported218 · Device fabrication method · Scheme 1
Solventacetonenot reported · cleaning solvent218 · Device fabrication method · Scheme 1
Solvent2-propanolnot reported · cleaning solvent218 · Device fabrication method · Scheme 1
Solventdistilled waternot reported · cleaning solvent218 · Device fabrication method · Scheme 1
OtherCo-CPnot reported · spin-coated thin film218 · Device fabrication method · Scheme 1
OtherAlnot reported · vacuum-deposited metallic contact218 · Device fabrication method · Scheme 1
Partial recipeSource: SI

Route 2: Liquid Liquid Interface

2-3 · Synthesis of compound Co-CP

Metal precursorsCo(NO3)2·6H2O (0.058 g, 0.2 mmol)
Linker precursorsbpd (0.042 g, 0.2 mmol); Hnac (0.023 g, 0.2 mmol)
SolventsMeOH, H2O, 1:1 MeOH/H2O buffer solution, EtOH
AdditivesEt3N (0.021 g, 0.2 mmol) to neutralise Hnac
Atmospherenot reported
Temperaturenot reported; crystallisation apparently at ambient temperature
Time72
Oxidant / reductantnone reported
Work-upbrown block-shaped crystals obtained after three days; washing/drying not reported
Activationnone reported
Scalability contextLayering crystallisation at millimole scale; no scale-up discussed.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linkerbpd0.042 g, 0.2 mmol · in MeOH (2 mL)2-3 · Synthesis of compound Co-CP
Metal SourceCo(NO3)2·6H2O0.058 g, 0.2 mmol · in H2O (2 mL)2-3 · Synthesis of compound Co-CP
SolventMeOH/H2O buffer solution2 mL · 1:1 v/v2-3 · Synthesis of compound Co-CP
LinkerHnac0.023 g, 0.2 mmol · in 2 mL EtOH2-3 · Synthesis of compound Co-CP
BaseEt3N0.021 g, 0.2 mmol · with Hnac in 2 mL EtOH2-3 · Synthesis of compound Co-CP
Partial recipeSource: Main

Route 3: Other

218 · Device fabrication method · Scheme 1

Metal precursorspre-synthesised Cu-CP
Linker precursorsnot applicable after CP synthesis
Solventsacetone, 2-propanol and distilled water used for ITO cleaning; coating dispersion solvent not reported
Additivesaluminium top contact
Atmospherevacuum oven drying; Al deposition at 4.7 x 10^-6 torr
Temperaturenot reported
Time1 h vacuum drying
Substrate orientationITO-coated glass substrate
Oxidant / reductantnone reported
Work-upspin-coated film dried in vacuum oven, then Al deposited through quad punch-hole shadow mask
Activationvacuum oven for 1 h
Scalability contextDevice area controlled by shadow mask; spin speed, film thickness and light intensity not reported.
Show 6 structured reagent records
RoleReagentAmount / concentrationSource
OtherITO-coated glass substratenot reported218 · Device fabrication method · Scheme 1
Solventacetonenot reported · cleaning solvent218 · Device fabrication method · Scheme 1
Solvent2-propanolnot reported · cleaning solvent218 · Device fabrication method · Scheme 1
Solventdistilled waternot reported · cleaning solvent218 · Device fabrication method · Scheme 1
OtherCu-CPnot reported · spin-coated thin film218 · Device fabrication method · Scheme 1
OtherAlnot reported · vacuum-deposited metallic contact218 · Device fabrication method · Scheme 1
Partial recipeSource: SI

Route 4: Liquid Liquid Interface

3 · Synthesis of compound Cu-CP

Metal precursorsCu(NO3)2·3H2O (0.048 g, 0.2 mmol)
Linker precursorsbpd (0.042 g, 0.2 mmol); Hnac (0.023 g, 0.2 mmol)
SolventsMeOH, H2O, 1:1 CH3CN/H2O buffer solution, EtOH
AdditivesEt3N (0.021 g, 0.2 mmol) to neutralise Hnac
Atmospherenot reported
Temperaturenot reported; crystallisation apparently at ambient temperature
Time120
Oxidant / reductantnone reported
Work-upgreen block-shaped crystals obtained after five days; washing/drying not reported
Activationnone reported
Scalability contextLayering crystallisation at millimole scale; no scale-up discussed.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linkerbpd0.042 g, 0.2 mmol · in MeOH (2 mL)3 · Synthesis of compound Cu-CP
Metal SourceCu(NO3)2·3H2O0.048 g, 0.2 mmol · in H2O (2 mL)3 · Synthesis of compound Cu-CP
SolventCH3CN/H2O buffer solution2 mL · 1:1 v/v3 · Synthesis of compound Cu-CP
LinkerHnac0.023 g, 0.2 mmol · in 2 mL EtOH3 · Synthesis of compound Cu-CP
BaseEt3N0.021 g, 0.2 mmol · with Hnac in 2 mL EtOH3 · Synthesis of compound Cu-CP