cMOF Evidence Base

Synthesis evidence

Redox-Active Ni(II) Nodes Induced Electrochromism in a Two-Dimensional Conductive Metal-Organic Framework

Pan L., Li R., Zhang C. et al. · ACS Applied Electronic Materials · 2022 · 2915-2922

9 structured synthesis routes

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

Complete recipeSource: Both

Route 1: Other

p006 · Experimental Section 4.5 · Scheme S3

Metal precursorsAu electrodes deposited on SiO2/Si substrate
SolventsDetergent, deionised water, acetone, ethanol
AtmosphereNitrogen drying flow; ambient measurement
Substrate orientationSiO2/Si wafer with pair of 80 nm Au electrodes; film transferred as for FTO electrode.
Work-upAu electrodes partially exposed by scraping off the film loaded on Au electrodes with tweezers before I-V measurement.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherAu electrodes80 nm thicknessp006 · Experimental Section 4.5 · Scheme S3
Solventdeionized waterNot specifiedp006 · Experimental Section 4.5 · Scheme S3
SolventacetoneNot specifiedp006 · Experimental Section 4.5 · Scheme S3
SolventethanolNot specifiedp006 · Experimental Section 4.5 · Scheme S3
AdditivedetergentNot specifiedp006 · Experimental Section 4.5 · Scheme S3
Complete recipeSource: Both

Route 2: Other

p005 · Experimental Section 4.4 · Figure 4a, Scheme S4

Solvents1 M LiClO4/propylene carbonate electrolyte
AdditivesScotch tape spacer and UV curing glue
Substrate orientationNi3(HITP)2 electrode cut into 2.5 x 2.5 cm2 pieces; Scotch tape spacer between Ni3(HITP)2 electrode and FTO glass.
Work-up1 M LiClO4/PC electrolyte injected into the spacer; injection ports sealed with UV curing glue.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
ElectrolyteLiClO4/PC4 mL · 1 Mp005 · Experimental Section 4.4 · Figure 4a, Scheme S4
AdditiveUV curing glue1.5 mLp005 · Experimental Section 4.4 · Figure 4a, Scheme S4
AdditiveScotch tape spacer0.3 cm thicknessp005 · Experimental Section 4.4 · Figure 4a, Scheme S4
OtherFTO glass counter electrodeNot specifiedp005 · Experimental Section 4.4 · Figure 4a, Scheme S4
Complete recipeSource: Both

Route 3: Air Liquid Interface

p005 · Experimental Section 4.2 · Scheme S1

Metal precursorsNickel(II) chloride hexahydrate (NiCl2.6H2O)
Linker precursorsHATP.6HCl
Solvents50 mL H2O
Additives0.3 mL aqueous ammonium hydroxide (NH3.H2O), 25% aqueous solution
Atmosphereair; liquid-air interface
Temperature50
Timefew minutes for visible dark-blue film formation; no total growth time specified
Substrate orientationFilm forms at liquid-air interface in cylindrical glassware, inner diameter 6 cm; later transferred horizontally to substrate.
Work-upFilm transferred to FTO; electrode rinsed with deionised water and methanol.
ActivationDried at 100 C in a vacuum oven for 24 h after transfer.
Scalability contextThickness was tuned by reactant concentration; larger-area uniform films were reported qualitatively by SEM.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O0.015 mmolp005 · Experimental Section 4.2 · Scheme S1
LinkerHATP.6HCl0.011 mmolp005 · Experimental Section 4.2 · Scheme S1
SolventH2O50 mLp005 · Experimental Section 4.2 · Scheme S1
Baseaqueous ammonium hydroxide (NH3.H2O)0.3 mL · 25% aqueous solutionp005 · Experimental Section 4.2 · Scheme S1
Complete recipeSource: Both

Route 4: Air Liquid Interface

p005 · Experimental Section 4.2 · Scheme S1

Metal precursorsNiCl2.6H2O, 4/3 times the 205 nm reactant amount
Linker precursorsHATP.6HCl, 4/3 times the 205 nm reactant amount
Solvents50 mL H2O; same procedure as 205 nm film
AdditivesAqueous ammonium hydroxide injection; same procedure as 205 nm film
Atmosphereair; liquid-air interface
Temperature50
Timefew minutes for visible dark-blue film formation; no total growth time specified
Substrate orientationLiquid-air interface film transferred to FTO by Langmuir-Schaefer method.
Work-upRinsed with DI water and methanol.
ActivationDried at 100 C in a vacuum oven for 24 h.
Scalability contextThe exact scaled Ni and linker quantities are implied by 4/3 scaling from 0.015 and 0.011 mmol.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O4/3 x 0.015 mmolp005 · Experimental Section 4.2 · Scheme S1
LinkerHATP.6HCl4/3 x 0.011 mmolp005 · Experimental Section 4.2 · Scheme S1
SolventH2O50 mLp005 · Experimental Section 4.2 · Scheme S1
Baseaqueous ammonium hydroxide (NH3.H2O)0.3 mL, same procedure · 25% aqueous solutionp005 · Experimental Section 4.2 · Scheme S1
Complete recipeSource: Both

Route 5: Air Liquid Interface

p005 · Experimental Section 4.2 · Scheme S1

Metal precursorsNiCl2.6H2O, 5/3 times the 205 nm reactant amount
Linker precursorsHATP.6HCl, 5/3 times the 205 nm reactant amount
Solvents50 mL H2O; same procedure as 205 nm film
AdditivesAqueous ammonium hydroxide injection; same procedure as 205 nm film
Atmosphereair; liquid-air interface
Temperature50
Timefew minutes for visible dark-blue film formation; no total growth time specified
Substrate orientationLiquid-air interface film transferred to FTO by Langmuir-Schaefer method.
Work-upRinsed with DI water and methanol.
ActivationDried at 100 C in a vacuum oven for 24 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O5/3 x 0.015 mmolp005 · Experimental Section 4.2 · Scheme S1
LinkerHATP.6HCl5/3 x 0.011 mmolp005 · Experimental Section 4.2 · Scheme S1
SolventH2O50 mLp005 · Experimental Section 4.2 · Scheme S1
Baseaqueous ammonium hydroxide (NH3.H2O)0.3 mL, same procedure · 25% aqueous solutionp005 · Experimental Section 4.2 · Scheme S1
Complete recipeSource: Both

Route 6: Air Liquid Interface

p005 · Experimental Section 4.2 · Scheme S1

Metal precursorsNiCl2.6H2O, 2 times the 205 nm reactant amount
Linker precursorsHATP.6HCl, 2 times the 205 nm reactant amount
Solvents50 mL H2O; same procedure as 205 nm film
AdditivesAqueous ammonium hydroxide injection; same procedure as 205 nm film
Atmosphereair; liquid-air interface
Temperature50
Timefew minutes for visible dark-blue film formation; no total growth time specified
Substrate orientationLiquid-air interface film transferred to FTO by Langmuir-Schaefer method.
Work-upRinsed with DI water and methanol.
ActivationDried at 100 C in a vacuum oven for 24 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O2 x 0.015 mmolp005 · Experimental Section 4.2 · Scheme S1
LinkerHATP.6HCl2 x 0.011 mmolp005 · Experimental Section 4.2 · Scheme S1
SolventH2O50 mLp005 · Experimental Section 4.2 · Scheme S1
Baseaqueous ammonium hydroxide (NH3.H2O)0.3 mL, same procedure · 25% aqueous solutionp005 · Experimental Section 4.2 · Scheme S1
Complete recipeSource: Both

Route 7: Air Liquid Interface

p005 · Experimental Section 4.2 · Scheme S1

Metal precursorsNiCl2.6H2O, 7/3 times the 205 nm reactant amount
Linker precursorsHATP.6HCl, 7/3 times the 205 nm reactant amount
Solvents50 mL H2O; same procedure as 205 nm film
AdditivesAqueous ammonium hydroxide injection; same procedure as 205 nm film
Atmosphereair; liquid-air interface
Temperature50
Timefew minutes for visible dark-blue film formation; no total growth time specified
Substrate orientationLiquid-air interface film transferred to FTO by Langmuir-Schaefer method.
Work-upRinsed with DI water and methanol.
ActivationDried at 100 C in a vacuum oven for 24 h.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O7/3 x 0.015 mmolp005 · Experimental Section 4.2 · Scheme S1
LinkerHATP.6HCl7/3 x 0.011 mmolp005 · Experimental Section 4.2 · Scheme S1
SolventH2O50 mLp005 · Experimental Section 4.2 · Scheme S1
Baseaqueous ammonium hydroxide (NH3.H2O)0.3 mL, same procedure · 25% aqueous solutionp005 · Experimental Section 4.2 · Scheme S1
Partial recipeSource: SI

Route 8: Other

S-5 / p005 · Supporting Scheme S4 · Scheme S4

AdditivesGlass mask
Substrate orientationGlass mask with number 8 pattern placed over Ni3(HITP)2 film/FTO.
Work-upLaser cut glass mask to obtain designated pattern; Ni3(HITP)2 electrode etched according to the glass mask to obtain the number 8 pattern.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Otherglass maskNot specifiedS-5 / p005 · Supporting Scheme S4 · Scheme S4
Complete recipeSource: Both

Route 9: Other

p005 · Experimental Section 4.3 · Scheme S1

SolventsDeionised water, acetone, ethanol for substrate cleaning; water bath for transfer; DI water and methanol rinse
AdditivesDetergent for substrate cleaning
AtmosphereNitrogen drying flow; vacuum oven after transfer
Temperature100
Time24
Substrate orientationFTO sunk horizontally and held up to the film in a bottle of water to transfer the film to the conductive side.
Work-upFTO cleaned ultrasonically in detergent, deionised water, acetone, and ethanol; electrode rinsed with DI water and methanol.
Activation100 C vacuum oven for 24 h
Scalability contextGeneral transfer route applies to FTO and SiO2/Si substrates.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Solventdeionized waterNot specifiedp005 · Experimental Section 4.3 · Scheme S1
Solventacetone95%p005 · Experimental Section 4.3 · Scheme S1
Solventethanol95%p005 · Experimental Section 4.3 · Scheme S1
Solventmethanolanalytical purityp005 · Experimental Section 4.3 · Scheme S1
AdditivedetergentNot specifiedp005 · Experimental Section 4.3 · Scheme S1