cMOF Evidence Base

Synthesis evidence

Li-TFSI endohedral Metal-Organic frameworks in stable perovskite solar cells for Anti-Deliquescent and restricting ion migration

Wang J., Zhang J., Yang Y. et al. · Chemical Engineering Journal · 2022 · 132481

7 structured synthesis routes

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

Partial recipeSource: Main

Route 1: Drop Cast

7 · Experimental section · Device fabrication

Metal precursorsnone
Linker precursorsnone
Solventschlorobenzene; acetonitrile carrier for Li-TFSI stock
AdditivesLi-TFSI; tBP
Atmosphereambient processing implied; not fully specified
Temperaturenot specified for HTL spin coating
Time20 s spin coating
Substrate orientationspin-coated on perovskite/device substrate
Oxidant / reductantambient oxygen participates in Spiro-OMeTAD oxidation according to discussion
Work-upspin-coated at 4000 rpm for 20 s
Activationnone after film formation reported
Scalability contextStandard solution-processed HTL control.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherSpiro-OMeTAD72.3 mg mL-1 in chlorobenzene · 72.3 mg mL-17 · Experimental section · Device fabrication
AdditiveLi-TFSI17.5 uL stock · 520 mg mL-1 in acetonitrile; 9.1 mg mL-1 final7 · Experimental section · Device fabrication
AdditivetBP29 uL7 · Experimental section · Device fabrication
Solventchlorobenzenenot specified7 · Experimental section · Device fabrication
Partial recipeSource: Main

Route 2: Drop Cast

7 · Experimental section · Device fabrication

Metal precursorsFe nodes only as preformed Li-TFSI@NH2-MIL-101 particles
Linker precursors2-aminoterephthalate only as preformed MOF particles
Solventschlorobenzene
AdditivestBP; Li-TFSI@NH2-MIL-101
Atmosphereambient processing implied; not fully specified
Temperaturenot specified for HTL spin coating
Time20 s spin coating
Substrate orientationspin-coated on perovskite/device substrate
Oxidant / reductantambient oxygen participates in Spiro-OMeTAD oxidation according to discussion
Work-upspin-coated at 4000 rpm for 20 s for conventional HTL; target spin parameters inferred same context but not explicitly restated
Activationnone after film formation reported
Scalability contextSolution processable HTL fabrication.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherSpiro-OMeTAD72.3 mg7 · Experimental section · Device fabrication
AdditivetBP29 uL7 · Experimental section · Device fabrication
AdditiveLi-TFSI@NH2-MIL-10115 mg · 15 mg mL-1 in chlorobenzene7 · Experimental section · Device fabrication
Solventchlorobenzene1 mL7 · Experimental section · Device fabrication
Partial recipeSource: Main

Route 3: Other

7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101

Metal precursorsactivated NH2-MIL-101 host contains Fe nodes
Linker precursorsactivated NH2-MIL-101 host contains 2-aminoterephthalate linkers
Solventsacetonitrile for Li-TFSI solution; acetonitrile and ethanol washes
AdditivesLi-TFSI solution (520 mg mL-1 in acetonitrile)
Atmospherenot specified
Temperatureroom temperature stirring; drying oven temperature not specified
Time36
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upexcess Li-TFSI solution removed by centrifugation; composite washed with acetonitrile and ethanol; dried in oven
ActivationNH2-MIL-101 pre-activated at 70 C for 24 h
Scalability contextPost-synthetic infiltration; mass of activated NH2-MIL-101 used is not specified in main text.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Otheractivated NH2-MIL-101not specified7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
AdditiveLi-TFSIexcessive solution · 520 mg mL-1 in acetonitrile7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
Solventacetonitrilenot specified7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
Solventethanolwash7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
Partial recipeSource: Main

Route 4: Drop Cast

7 · Experimental section · Device fabrication

Metal precursorsFe nodes only as preformed NH2-MIL-101 particles
Linker precursors2-aminoterephthalate only as preformed NH2-MIL-101 particles
Solventschlorobenzene
AdditivesLi-TFSI; NH2-MIL-101 physical mixture; tBP
Atmosphereambient processing implied; not fully specified
Temperaturenot specified for HTL spin coating
Timenot specified for this control HTL
Substrate orientationspin-coated on perovskite/device substrate
Oxidant / reductantambient oxygen participates in Spiro-OMeTAD oxidation according to discussion
Work-upprepared as an HTL solution; spin-coating parameters for this specific control are not restated
Activationnone after film formation reported
Scalability contextSolution-processed physical-mixture HTL control.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
OtherSpiro-OMeTAD72.3 mg7 · Experimental section · Device fabrication
AdditivetBP29 uL7 · Experimental section · Device fabrication
AdditiveLi-TFSI2.01 mg7 · Experimental section · Device fabrication
OtherNH2-MIL-10112.99 mg7 · Experimental section · Device fabrication
Solventchlorobenzene1 mL7 · Experimental section · Device fabrication
Partial recipeSource: Main

Route 5: Hydrothermal

7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101

Metal precursorsFeCl3.6H2O (2.492 g, 9.22 mmol)
Linker precursors2-Aminoterephthalic acid (1.670 g, 9.22 mmol)
Solventsdimethylformamide (DMF, 200 mL)
Atmospherenot specified
Temperature150
Time0.5
Substrate orientationnot applicable
Oxidant / reductantnone specified
Work-upcollected by centrifugation at 12000 rpm for 10 min, then washed with DMF and ethanol sequentially
Activationheated at 70 C for 24 h
Scalability contextRapid 30 min reaction in 200 mL DMF; no yield reported in main text.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceFeCl3.6H2O2.492 g, 9.22 mmol7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
Linker2-Aminoterephthalic acid1.670 g, 9.22 mmol7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
Solventdimethylformamide (DMF)200 mL7 · Experimental section · Synthesis of NH2-MIL-101 and Li-TFSI@NH2-MIL-101
Partial recipeSource: Main

Route 6: Drop Cast

7 · Experimental section · Device fabrication

Metal precursorsPbI2, PbBr2, CsI; titanium(IV) isopropanol for compact TiO2
Linker precursorsFAI and MABr organic cation salts; PC61BM electron transport material
SolventsDMF/DMSO 4:1 for perovskite; isopropanol for TiO2; chlorobenzene antisolvent and PC61BM solvent
AdditivesLi-TFSI@NH2-MIL-101 doped Spiro-OMeTAD HTL; tBP
Atmospherenot specified
TemperatureTiO2 sintered 500 C; PC61BM heated 70 C; perovskite annealed 100 C
TimeTiO2 30 min; PC61BM 10 min; perovskite 1 h
Substrate orientationFTO glass etched with zinc powder/3 M HCl; UV ozone 15 min
Oxidant / reductantnone specified
Work-upsequential spin coating; 200 uL chlorobenzene antisolvent in last 5 s; Au 80 nm thermally evaporated
ActivationUV ozone substrate treatment
Scalability contextSmall-area devices, active area 0.06 cm2.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2not specified · part of 1.2 M perovskite precursor7 · Experimental section · Device fabrication
Metal SourcePbBr2not specified · part of 1.2 M perovskite precursor7 · Experimental section · Device fabrication
AdditiveCsInot specified · 390 mg mL-1 in DMSO stock7 · Experimental section · Device fabrication
OtherFAInot specified7 · Experimental section · Device fabrication
OtherMABrnot specified7 · Experimental section · Device fabrication
SolventDMF/DMSO1 mL · volume ratio 4:17 · Experimental section · Device fabrication
OtherPC61BMnot specified · 5 mg mL-1 in chlorobenzene7 · Experimental section · Device fabrication
Othertitanium(IV) isopropanol175 uL · in 2.5 mL isopropanol7 · Experimental section · Device fabrication
Partial recipeSource: Main

Route 7: Drop Cast

7 · Experimental section · Device fabrication

Metal precursorsnone
Linker precursorsnone
Solventschlorobenzene
AdditivesLi-TFSI; tBP
Atmosphereambient processing implied; not fully specified
Temperaturenot specified for HTL spin coating
Timenot specified for this control HTL
Substrate orientationspin-coated on perovskite/device substrate
Oxidant / reductantambient oxygen participates in Spiro-OMeTAD oxidation according to discussion
Work-upprepared as an HTL solution; spin-coating parameters for this specific control are not restated
Activationnone after film formation reported
Scalability contextSolution-processed low-Li-TFSI HTL control.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
OtherSpiro-OMeTAD72.3 mg7 · Experimental section · Device fabrication
AdditivetBP29 uL7 · Experimental section · Device fabrication
AdditiveLi-TFSI2.01 mg · 2.01 mg mL-1 in chlorobenzene7 · Experimental section · Device fabrication
Solventchlorobenzene1 mL7 · Experimental section · Device fabrication