cMOF Evidence Base

Synthesis evidence

Regulating Crystallization and Lead Leakage of Perovskite Solar Cell Via Novel Polyoxometalate-Based Metal–Organic Framework

Dong Y., Zhang J., Wang W. et al. · Small · 2023 · 2301824

4 structured synthesis routes

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

Complete recipeSource: SI

Route 1: Other

p002 · Device Fabrication

Metal precursorsPbI2 (1.54 M, 10% excess), PbBr2 (0.06 M), CsPbI3 (0.045 M)
Linker precursorsFAI (1.4 M), MABr (0.06 M), MACl (0.5 M), oFPEAI passivation layer, Spiro-OMeTAD HTM
SolventsDMF/DMSO (8:1 v/v), chlorobenzene antisolvent, isopropanol, acetonitrile, CB/CN for HTM dopants
AdditivesMACl; oFPEAI; TBP, Li-TFSI, FK209 in HTM
Atmospherenitrogen-filled glove box for perovskite annealing; air for J-V/EIS measurements
Temperature120 for perovskite anneal; 100 for oFPEAI anneal; 500 for TiO2 sintering
Time1 for perovskite anneal; 0.083 for oFPEAI anneal; 0.5 for TiO2 sintering
Substrate orientationPlanar FTO/ETL/perovskite/HTL/Au
Work-upFTO etched with 3 M HCl/Zn, cleaned by sonication, ozone-treated; TiO2 spin-coated and sintered; perovskite spin-coated 1000/5000 rpm; chlorobenzene antisolvent; HTM spin-coated; about 80 nm Au evaporated.
ActivationAnnealed perovskite at 120 degC for 1 h in nitrogen glove box.
Scalability contextLab-scale spin-coated planar PSC; active area 0.06 cm2.
Show 13 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI21.54 M, 10% excess PbI2p002 · Device Fabrication
Metal SourcePbBr20.06 Mp002 · Device Fabrication
Metal SourceCsPbI30.045 Mp002 · Device Fabrication
OtherFAI1.4 Mp002 · Device Fabrication
OtherMABr0.06 Mp002 · Device Fabrication
AdditiveMACl0.5 Mp002 · Device Fabrication
SolventDMF/DMSO1 mL · 8:1 v/vp002 · Device Fabrication
Solventchlorobenzene150 uLp002 · Device Fabrication
AdditiveoFPEAI20 mM in isopropanolp002 · Device Fabrication
AdditiveSpiro-OMeTAD72.3 mg · in 1 mL CBp002 · Device Fabrication
AdditiveTBP29 uLp002 · Device Fabrication
AdditiveLi-TFSI17.5 uL solution · 520 mg in 1 mL acetonitrilep002 · Device Fabrication
AdditiveFK20930 uL solution · 300 mg in 1 mL CNp002 · Device Fabrication
Partial recipeSource: Main

Route 2: Other

p002 · 2.1 Structure and Properties of POMOF · Figure S5b

Metal precursorsPOMOF from route_pomof_solvothermal
Atmospherenot specified
Temperature300
Time12
Work-upThermal treatment to remove residual solvent and floating water molecules before device use.
ActivationHeated at 300 degC for 12 h.
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
OtherPOMOFnot specifiedp002 · 2.1 Structure and Properties of POMOF · Figure S5b
Complete recipeSource: Both

Route 3: Other

p002 · Preparation of Perovskite Precursor Solution

Metal precursorsSame triple-cation Pb-halide precursor as control plus activated POMOF additive
Linker precursorsPOMOF contains pyridine/imidazole; perovskite cations FAI, MABr, MACl, oFPEAI
SolventsDMF/DMSO (8:1 v/v), chlorobenzene containing POMOF, isopropanol, CB/CN/acetonitrile for HTM processing
AdditivesPOMOF in chlorobenzene; optimised 1.5 mg mL-1; oFPEAI; TBP, Li-TFSI, FK209
Atmospherenitrogen-filled glove box for perovskite annealing; air for J-V/EIS measurements
Temperature120 for perovskite anneal; 100 for oFPEAI anneal; 500 for TiO2 sintering
Time1 for perovskite anneal; 0.083 for oFPEAI anneal; 0.5 for TiO2 sintering
Substrate orientationPlanar FTO/ETL/perovskite-POMOF/HTL/Au
Oxidant / reductantPOMOF redox activity proposed to oxidise Pb0 defects; no external oxidant in film fabrication
Work-upPOMOF dispersed in chlorobenzene by ultrasonic cell disruptor, applied as antisolvent during last 15 s of perovskite spin-coating; subsequent anneal and HTL/Au deposition as control.
ActivationPOMOF preheated at 300 degC for 12 h; perovskite annealed at 120 degC for 1 h.
Scalability contextLab-scale spin-coated PSC; dose optimisation reported from 0.5 to 3 mg mL-1 POMOF.
Show 8 structured reagent records
RoleReagentAmount / concentrationSource
AdditivePOMOFnot specified in film route · 0.5, 1.0, 1.5, 2.0, 3.0 mg mL-1 tested; 1.5 mg mL-1 optimalp002 · Preparation of Perovskite Precursor Solution
Solventchlorobenzene150 uL antisolventp002 · Preparation of Perovskite Precursor Solution
Metal SourcePbI21.54 M, 10% excess PbI2p002 · Preparation of Perovskite Precursor Solution
Metal SourcePbBr20.06 Mp002 · Preparation of Perovskite Precursor Solution
Metal SourceCsPbI30.045 Mp002 · Preparation of Perovskite Precursor Solution
OtherFAI1.4 Mp002 · Preparation of Perovskite Precursor Solution
OtherMABr0.06 Mp002 · Preparation of Perovskite Precursor Solution
AdditiveMACl0.5 Mp002 · Preparation of Perovskite Precursor Solution
Complete recipeSource: SI

Route 4: Solvothermal

p001 · Methods - Synthesis of POMOF

Metal precursorsZn(OAc)2.4H2O (0.1098 g, 0.5 mmol); MoO3 (0.0719 g, 0.50 mmol)
Linker precursorsimidazole (0.068 g, 1.001 mmol); pyridine present in mixed solvent
Solventspyridine, ethyl alcohol (5 mL), deionized water (5 mL)
Additives85% concentrated phosphoric acid to pH 4.7
Atmospherenot specified
Temperature140
Time120
Work-upCool to room temperature; wash reddish-brown block crystals with ethyl alcohol; dry at room temperature; yield 35.26%.
ActivationNone in synthesis step; separate 300 degC/12 h pretreatment used before PSC application.
Scalability contextSmall batch in 20.0 mL Teflon-lined stainless-steel vessel.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceZn(OAC)2.4H2O0.1098 g, 0.5 mmolp001 · Methods - Synthesis of POMOF
Metal SourceMoO30.0719 g, 0.50 mmolp001 · Methods - Synthesis of POMOF
Linkerimidazole0.068 g, 1.001 mmolp001 · Methods - Synthesis of POMOF
Solventpyridinenot specifiedp001 · Methods - Synthesis of POMOF
Solventethyl alcohol5 mLp001 · Methods - Synthesis of POMOF
Solventdeionized water5 mLp001 · Methods - Synthesis of POMOF
Acidconcentrated phosphoric acidto pH 4.7 · 85%p001 · Methods - Synthesis of POMOF