Synthesis · Metal organic framework doped Spiro-OMeTAD with increased conductivity for improving perovskite solar cell performance

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

2 · 2.2. Device fabrication

Solventschlorobenzene, 1 mL; Li-TFSI stock in acetonitrile

Additives4-tert-butylpyridine (TBP), Li-TFSI

Atmospherenot reported

Temperatureroom temperature/not reported

Time24 h stirring; 20 s spin coating

Substrate orientationSpun onto perovskite layer in device fabrication

Oxidant / reductantLi-TFSI additive; no In10 oxidant

Work-upSpin coated at 4000 rpm for 20 s.

ActivationNo separate activation reported.

Scalability contextSpin-coated thin film process.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	Spiro-OMeTAD	72.9 mg	2 · 2.2. Device fabrication
Additive	4-tert-butylpyridine (TBP)	29 uL	2 · 2.2. Device fabrication
Additive	lithium bis(trifluoromethanesulfonyl)imide (Li-TFSI)	17.5 uL stock · 520 mg/mL in acetonitrile	2 · 2.2. Device fabrication
Solvent	chlorobenzene	1 mL	2 · 2.2. Device fabrication

Partial recipeSource: Main

Route 2: Other

2 · 2.2. Device fabrication

Metal precursorsIn10 MOF from route_in10_solvothermal_main

Linker precursorsIn10 MOF plus Spiro-OMeTAD matrix

Solventschlorobenzene HTM solution with Li-TFSI stock in acetonitrile

AdditivesIn10, TBP, Li-TFSI

Atmospherenot reported

Temperatureroom temperature/not reported

Time24 h stirring for base HTM solution; 20 s spin coating

Substrate orientationSpun onto perovskite layer in device fabrication

Oxidant / reductantIn10 acts as oxidising additive for Spiro-OMeTAD

Work-upSpin coated at 4000 rpm for 20 s.

ActivationNo separate activation reported.

Scalability contextSolution additive and spin-coated thin film process.

Show 5 structured reagent records

Role	Reagent	Amount / concentration	Source
Other	In10 MOF	2, 4, or 6 mg added · 2, 4, or 6 mg/mL in HTM solution	2 · 2.2. Device fabrication
Other	Spiro-OMeTAD	72.9 mg in base HTM solution	2 · 2.2. Device fabrication
Additive	4-tert-butylpyridine (TBP)	29 uL	2 · 2.2. Device fabrication
Additive	Li-TFSI	17.5 uL stock · 520 mg/mL in acetonitrile	2 · 2.2. Device fabrication
Solvent	chlorobenzene	1 mL	2 · 2.2. Device fabrication

Partial recipeSource: Main

Route 3: Solvothermal

2 · 2.1. Synthesis of In10

Metal precursorsIndium chloride (InCl3), 0.0442 g; potassium hydroxide used for pH adjustment

Linker precursorsquinoline-3-dicarboxylic acid (3-H2qldc), 0.0220 g

Solventsacetonitrile, 8 mL

Additivespotassium hydroxide to pH 6.5

Atmospherenot reported

Temperature120

Time120

Work-upCooled to room temperature; white precipitate washed with water.

ActivationDried at room temperature; no activation procedure reported.

Scalability contextBatch synthesis in stainless-steel autoclave; reported isolated yield 71.2%.

Show 4 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	indium chloride (InCl3)	0.0442 g	2 · 2.1. Synthesis of In10
Linker	quinoline-3-dicarboxylic acid (3-H2qldc)	0.0220 g	2 · 2.1. Synthesis of In10
Solvent	acetonitrile	8 mL	2 · 2.1. Synthesis of In10
Base	potassium hydroxide	to pH 6.5	2 · 2.1. Synthesis of In10

Partial recipeSource: Main

Route 4: Other

2 · 2.2. Device fabrication

Metal precursorsPbI2, PbBr2, Ti precursor, CsI; In10 MOF in HTM for doped devices

Linker precursorsformamidinium iodide and methylammonium bromide for perovskite; Spiro-OMeTAD HTM

SolventsDMF/DMSO (4:1 v/v), isopropanol, chlorobenzene, acetonitrile stock

AdditivesCsI, TBP, Li-TFSI, In10 for doped HTM devices

Atmospherenot reported

Temperature500 degC TiO2 roast; 70 degC precursor stirring; 100 degC perovskite anneal

Time10 min oxygen plasma; 30 s TiO2 spin; 30 min TiO2 roast; 24 h perovskite precursor stirring; 10 s/30 s perovskite spin; 15 min anneal; 20 s HTM spin

Substrate orientationFTO glass etched and coated with TiO2, perovskite, HTM/In10 and Au

Oxidant / reductantIn10 oxidises Spiro-OMeTAD in doped HTM devices

Work-upAu electrode evaporated under vacuum.

ActivationNo separate device activation reported.

Scalability contextLaboratory spin-coated PSC device stack; active cell area 0.06 cm2 for measurements.

Show 7 structured reagent records

Role	Reagent	Amount / concentration	Source
Metal Source	lead iodide	1.1 mmol	2 · 2.2. Device fabrication
Metal Source	lead bromide	0.22 mmol	2 · 2.2. Device fabrication
Other	formamidinium iodide	1 mmol	2 · 2.2. Device fabrication
Other	methylammonium bromide	0.2 mmol	2 · 2.2. Device fabrication
Solvent	N,N-dimethylformamide/dimethyl sulfoxide	1 mL mixture · 4:1 v/v	2 · 2.2. Device fabrication
Additive	cesium iodide	42 uL · 1.5 M in DMSO	2 · 2.2. Device fabrication
Other	Au	70-80 nm evaporated	2 · 2.2. Device fabrication