Synthesis evidence

Conductive Ni3(HITP)2 nanofilm with asymmetrical morphology prepared by gas–liquid interface self-assembly for glucose sensing

Cao L.-A., Wei M., Guo X. et al. · Ionics · 2024 · 2375-2385

8 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

p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements

Metal precursorspreformed Ni3(HITP)2 film
Solventsacetone, isopropanol, ethanol for ITO rinsing
Atmospheredried under a flow of air
Temperatureroom temperature
Substrate orientationITO substrate (1 x 1 cm2); stamping transfer; ~10 nm film from growth-time series
Work-upITO rinsed with acetone, isopropanol and ethanol; dried; Ni3(HITP)2 film transferred by stamping
ActivationBefore electrochemical tests, CV activation from 0.2 to 0.8 V vs Ag/AgCl at 50 mV s^-1 for 50 cycles in 0.1 M NaOH until stable.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial ITO substrate1 x 1 cm2p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Solventacetone, isopropanol, ethanolNot specifiedp003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Complete recipeSource: Main

Route 2: Other

p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements

Metal precursorspreformed Ni3(HITP)2 film
Solventsacetone, isopropanol, ethanol for ITO rinsing
Atmospheredried under a flow of air
Temperatureroom temperature
Substrate orientationITO substrate (1 x 1 cm2); stamping transfer; ~100 nm film from growth-time series
Work-upITO rinsed with acetone, isopropanol and ethanol; dried; Ni3(HITP)2 film transferred by stamping
ActivationBefore electrochemical tests, CV activation from 0.2 to 0.8 V vs Ag/AgCl at 50 mV s^-1 for 50 cycles in 0.1 M NaOH until stable.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial ITO substrate1 x 1 cm2p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Solventacetone, isopropanol, ethanolNot specifiedp003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Complete recipeSource: Main

Route 3: Other

p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements

Metal precursorspreformed Ni3(HITP)2 film
Solventsacetone, isopropanol, ethanol for ITO rinsing
Atmospheredried under a flow of air
Temperatureroom temperature
Substrate orientationITO substrate (1 x 1 cm2); stamping transfer exposes down-side surface
Work-upITO rinsed with acetone, isopropanol and ethanol; dried; Ni3(HITP)2 film transferred by stamping
ActivationBefore electrochemical tests, CV activation from 0.2 to 0.8 V vs Ag/AgCl at 50 mV s^-1 for 50 cycles in 0.1 M NaOH until stable.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial ITO substrate1 x 1 cm2p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Solventacetone, isopropanol, ethanolNot specifiedp003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Complete recipeSource: Main

Route 4: Other

p002 / 2376 · Preparation of HITP ligand

Linker precursorsN,N',N'',N''',N'''',N'''''-(triphenylene-2,3,6,7,10,11-hexayl) hexakis(1,1-diphenylmethanimine), 219 mg (0.18 mmol)
Solventstetrahydrofuran, 10 mL
Additives2 M HCl, 1 mL
Atmospherenot reported
Temperatureroom temperature
Time0.5
Work-upcentrifuging, washing and drying
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
LinkerN, N', N'', N''', N'''', N'''''-(triphenylene-2,3,6,7,10,11-hexayl) hexakis (1,1-diphenylmethanimine)219 mg (0.18 mmol)p002 / 2376 · Preparation of HITP ligand
Solventtetrahydrofuran10 mLp002 / 2376 · Preparation of HITP ligand
AcidHCl1 mL · 2 Mp002 / 2376 · Preparation of HITP ligand
Complete recipeSource: Main

Route 5: Air Liquid Interface

p002-p003 / 2376-2377 · Preparation of Ni3(HITP)2 film · Fig. 1

Metal precursorsNiCl2.6H2O, 9.0 mg in 10 mL deionized water
Linker precursorsHITP.6HCl, 10 mg in 10 mL deionized water
Solventsdeionized water
Additivesammonia water, 0.4 mL
Atmosphereair-liquid interface; gas atmosphere otherwise not specified
Temperature65
Time0.0167-0.0833
Substrate orientationFilm formed at air-liquid interface; later transferred to substrates.
Work-upmixed precursor solutions were sonicated 10 min, heated in oil bath, film transferred onto substrates
Scalability contextFilm thickness controlled in nanometre scale by reaction time from 1 to 5 min.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O9.0 mg · dissolved in 10 mL deionized waterp002-p003 / 2376-2377 · Preparation of Ni3(HITP)2 film · Fig. 1
LinkerHITP.6HCl10 mg · dissolved in 10 mL deionized waterp002-p003 / 2376-2377 · Preparation of Ni3(HITP)2 film · Fig. 1
Solventdeionized water10 mL for each precursor solutionp002-p003 / 2376-2377 · Preparation of Ni3(HITP)2 film · Fig. 1
Baseammonia water0.4 mLp002-p003 / 2376-2377 · Preparation of Ni3(HITP)2 film · Fig. 1
Complete recipeSource: Main

Route 6: Other

p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements

Metal precursorspreformed Ni3(HITP)2 film
Solventsacetone, isopropanol, ethanol for ITO rinsing
Atmospheredried under a flow of air
Temperatureroom temperature
Substrate orientationITO substrate (1 x 1 cm2); salvaging transfer; ~10 nm film from growth-time series
Work-upITO rinsed with acetone, isopropanol and ethanol; dried; Ni3(HITP)2 film transferred by salvaging
ActivationBefore electrochemical tests, CV activation from 0.2 to 0.8 V vs Ag/AgCl at 50 mV s^-1 for 50 cycles in 0.1 M NaOH until stable.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial ITO substrate1 x 1 cm2p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Solventacetone, isopropanol, ethanolNot specifiedp003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Complete recipeSource: Main

Route 7: Other

p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements

Metal precursorspreformed Ni3(HITP)2 film
Solventsacetone, isopropanol, ethanol for ITO rinsing
Atmospheredried under a flow of air
Temperatureroom temperature
Substrate orientationITO substrate (1 x 1 cm2); salvaging transfer; ~100 nm film from growth-time series
Work-upITO rinsed with acetone, isopropanol and ethanol; dried; Ni3(HITP)2 film transferred by salvaging
ActivationBefore electrochemical tests, CV activation from 0.2 to 0.8 V vs Ag/AgCl at 50 mV s^-1 for 50 cycles in 0.1 M NaOH until stable.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial ITO substrate1 x 1 cm2p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Solventacetone, isopropanol, ethanolNot specifiedp003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Complete recipeSource: Main

Route 8: Other

p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements

Metal precursorspreformed Ni3(HITP)2 film
Solventsacetone, isopropanol, ethanol for ITO rinsing
Atmospheredried under a flow of air
Temperatureroom temperature
Substrate orientationITO substrate (1 x 1 cm2); salvaging transfer exposes up-side surface
Work-upITO rinsed with acetone, isopropanol and ethanol; dried; Ni3(HITP)2 film transferred by salvaging
ActivationBefore electrochemical tests, CV activation from 0.2 to 0.8 V vs Ag/AgCl at 50 mV s^-1 for 50 cycles in 0.1 M NaOH until stable.
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial ITO substrate1 x 1 cm2p003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements
Solventacetone, isopropanol, ethanolNot specifiedp003 / 2377 · Preparation of Ni3(HITP)2 film/ITO electrode; Electrochemical measurements