Synthesis · Three-type precursors for low-temperature solution-processed void-and-crack-free copper(I) iodide films: comparison of electrical conductivities and optical transparency

9 structured synthesis routes

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

Partial recipeSource: Both

Route 1: Other

6 · 3.4 Fabrication of CuI thin films on FTO and PET substrates

Metal precursorsCuI-1A2P precursor solution

Linker precursors1-amino-2-propanol

Solvents2-methoxyethanol

Atmosphereambient air implied

Temperature150

Substrate orientationFTO glass substrate

Work-upCuI thin films fabricated on FTO using a 1A2P precursor solution; detailed spin-coating parameters not restated in the FTO section.

Activationheated, exact FTO heating time not restated in main-text FTO section

Scalability contextFTO particulates were completely covered using over 0.26 M 1A2P precursor solution.

Show 1 structured reagent record

Role	Reagent	Amount / concentration	Source
Metal Source	CuI-1A2P precursor solution	>0.26 M for complete coverage	6 · 3.4 Fabrication of CuI thin films on FTO and PET substrates

Complete recipeSource: Both

Route 2: Other

3 · 2.2 CuI film preparation · Fig. 1

Metal precursorsextra-pure grade CuI (95% purity)

Linker precursors1-amino-2-propanol (1A2P) alkanolamine precursor ligand

Solvents2-methoxyethanol (2ME)

Atmosphereambient air required for oxidation; dissolution did not occur in N2-filled glove box

Temperature150

Time1

Substrate orientationclean glass plate, 2.5 cm x 2.5 cm

Oxidant / reductantoxygen from ambient air oxidises Cu(I) to Cu(II) during alkanolamine complex formation

Work-upCuI reacted with 1A2P at alkanolamine/CuI = 5 mol/mol; concentration controlled at 0.13-0.70 mol L-1 with 2ME; sonicated to blue solution; used without filtration; 75 uL spin coated at 1000 rpm 10 s and 1500 rpm 30 s; heated.

Activationthermal decomposition at 150 deg C for 1 h

Scalability contextAuthors identify 1A2P as producing void-and-crack-free CuI films with controlled thickness over 50 nm.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	0.13 to 0.70 mol L-1	3 · 2.2 CuI film preparation · Fig. 1
Linker	1A2P	alkanolamine/CuI = 5 mol/mol	3 · 2.2 CuI film preparation · Fig. 1
Solvent	2ME	different volumes	3 · 2.2 CuI film preparation · Fig. 1
Oxidant	ambient oxygen	Not specified	3 · 2.2 CuI film preparation · Fig. 1

Complete recipeSource: Both

Route 3: Other

3 · 2.2 CuI film preparation

Metal precursorsCuI-1A2P complex precursor solution

Linker precursors1-amino-2-propanol

Solvents2-methoxyethanol

Atmosphereambient air implied

Temperature150

Time1

Substrate orientationclean PET substrate

Work-up0.26 M 2ME solution of CuI-1A2P complex, 75 uL, spin coated on PET at 1000 rpm 10 s then 1500 rpm 30 s.

Activationheated to 150 deg C for 1 h

Scalability contextDemonstrates compatibility with flexible PET substrate.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI-1A2P complex precursor	75 uL · 0.26 M	3 · 2.2 CuI film preparation
Solvent	2ME	Not specified	3 · 2.2 CuI film preparation

Complete recipeSource: Both

Route 4: Other

3 · 2.2 CuI film preparation · Fig. 1

Metal precursorsextra-pure grade CuI (95% purity)

Linker precursors2-aminoethanol (2AE) alkanolamine precursor ligand

Solvents2-methoxyethanol (2ME)

Atmosphereambient air required for oxidation; dissolution did not occur in N2-filled glove box

Temperature50-150

Time1

Substrate orientationclean glass plate, 2.5 cm x 2.5 cm

Oxidant / reductantoxygen from ambient air oxidises Cu(I) to Cu(II) during alkanolamine complex formation

Work-upCuI reacted with 2AE at alkanolamine/CuI = 5 mol/mol; concentration controlled at 0.13-0.70 mol L-1 with 2ME; sonicated to blue solution; used without filtration; 75 uL spin coated and heated.

Activationthermal decomposition by heating to 150 deg C for 1 h

Scalability context2AE precursor solution had low stability and was used immediately because blue precipitates formed within days.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	0.13 to 0.70 mol L-1	3 · 2.2 CuI film preparation · Fig. 1
Linker	2AE	alkanolamine/CuI = 5 mol/mol	3 · 2.2 CuI film preparation · Fig. 1
Solvent	2ME	different volumes	3 · 2.2 CuI film preparation · Fig. 1
Oxidant	ambient oxygen	Not specified	3 · 2.2 CuI film preparation · Fig. 1

Complete recipeSource: Both

Route 5: Other

3 · 2.2 CuI film preparation · Fig. 1

Metal precursorsextra-pure grade CuI (95% purity)

Linker precursors2-amino-2-methyl-1-propanol (2AM1P) alkanolamine precursor ligand

Solvents2-methoxyethanol (2ME)

Atmosphereambient air required for oxidation; dissolution did not occur in N2-filled glove box

Temperature150

Time1

Substrate orientationclean glass plate, 2.5 cm x 2.5 cm

Oxidant / reductantambient oxygen

Work-upCuI reacted with 2AM1P at alkanolamine/CuI = 5 mol/mol in 2ME; sonicated to blue solution; spin coated and heated using the same procedure as AN/DES precursor solutions.

Activationattempted thermal treatment at 150 deg C for 1 h

Scalability context2AM1P was rejected because the complex did not decompose to CuI at 150 deg C.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	0.13 to 0.70 mol L-1	3 · 2.2 CuI film preparation · Fig. 1
Linker	2AM1P	alkanolamine/CuI = 5 mol/mol	3 · 2.2 CuI film preparation · Fig. 1
Solvent	2ME	different volumes	3 · 2.2 CuI film preparation · Fig. 1

Complete recipeSource: Both

Route 6: Other

2 · 2.2 CuI film preparation

Metal precursorsextra-pure grade CuI (95% purity)

Linker precursorsnone

Solventsacetonitrile (AN)

Additiveshydrophobic PTFE membrane filter, 0.45 um pore size, for cloudy AN precursor

Atmospherenot specified; ambient implied

Temperature50-150

Time1

Substrate orientationclean glass plate, 2.5 cm x 2.5 cm

Work-upCuI dissolved in AN by sonication; cloudy AN precursor filtered; 75 uL spread by spin coating at 1000 rpm 10 s then 1500 rpm 30 s; heated.

Activationthermal treatment at varied temperatures between 50 and 150 deg C for 1 h

Scalability contextAN saturation to dissolve CuI is low and solutions are cloudy before filtration.

Show 3 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	0.13 to 0.70 mol L-1	2 · 2.2 CuI film preparation
Solvent	AN	Not specified	2 · 2.2 CuI film preparation
Other	PTFE membrane filter	0.45 um pore size	2 · 2.2 CuI film preparation

Complete recipeSource: Both

Route 7: Other

2 · 2.2 CuI film preparation

Metal precursorsextra-pure grade CuI (95% purity)

Linker precursorsnone

Solventsdiethyl sulfide (DES)

Atmospherenot specified; ambient implied

Temperature50-150

Time1

Substrate orientationclean glass plate, 2.5 cm x 2.5 cm

Work-upCuI dissolved in DES by sonication; 75 uL spread by spin coating at 1000 rpm 10 s then 1500 rpm 30 s; heated.

Activationthermal treatment at varied temperatures between 50 and 150 deg C for 1 h

Scalability contextDES dissolves CuI over 0.13-0.70 M but is described as unpleasant-smelling and expensive.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	CuI	0.13 to 0.70 mol L-1	2 · 2.2 CuI film preparation
Solvent	DES	Not specified	2 · 2.2 CuI film preparation

Complete recipeSource: Both

Route 8: Other

3 · 2.3 Isolation of CuI-1A2P and CuI-2AE complexes

Metal precursorsCuI-1A2P complex precursor solution

Linker precursors1-amino-2-propanol

Solvents2ME; toluene poor solvent

Atmosphereroom temperature, atmosphere not specified

Temperatureroom temperature

Time24

Work-upBlue 0.26 mol L-1 CuI-1A2P precursor solution (5 mL) diluted with toluene (15 mL), left 24 h at room temperature, centrifuged at 2600 x g and washed with toluene.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	CuI-1A2P complex precursor solution	5 mL · 0.26 mol L-1	3 · 2.3 Isolation of CuI-1A2P and CuI-2AE complexes
Solvent	toluene	15 mL	3 · 2.3 Isolation of CuI-1A2P and CuI-2AE complexes

Vague recipeSource: Both

Route 9: Other

3 · 2.3 Isolation of CuI-1A2P and CuI-2AE complexes

Metal precursorsCuI-2AE complex precursor solution

Linker precursors2-aminoethanol

Solvents2ME; toluene poor solvent inferred from similar method

Atmosphereroom temperature, atmosphere not specified

Temperatureroom temperature

Work-upPrepared using a similar method to isolated CuI-1A2P; exact volumes and concentrations not restated.

Show 2 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	CuI-2AE precursor solution	Not specified	3 · 2.3 Isolation of CuI-1A2P and CuI-2AE complexes
Solvent	toluene	Not specified	3 · 2.3 Isolation of CuI-1A2P and CuI-2AE complexes