cMOF Evidence Base

Synthesis evidence

Effect of solvent on the perovskite thin film morphology and crystallinity

Wang D., Zhu H.-M., Zhou Z.-M. et al. · Wuli Xuebao/Acta Physica Sinica · 2015 · 038403

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: Other

038403-2 · 2.3

Metal precursorsPbI2; TiO2 gel; commercial TiO2 paste
Linker precursorsMAI; spiro-MeOTAD
SolventsDMF; anhydrous ethanol; chlorobenzene
AdditivestBP; Li-TFSI
AtmosphereTiO2 calcined in air; perovskite coating/annealing in glovebox; spiro-MeOTAD oxidised in air
Temperature550 C TiO2 calcination; 100 C perovskite anneal
Time0.5 h compact TiO2 calcination; 0.5 h mesoporous TiO2 calcination; 0.5 h perovskite anneal; 12 h air oxidation
Substrate orientationetched FTO glass
Oxidant / reductantair oxidation of spiro-MeOTAD
Work-upFTO etched with zinc powder and 3% HCl, ultrasonically cleaned with deionised water, acetone, and anhydrous ethanol; compact TiO2 and mesoporous TiO2 deposited and calcined; MAPbI3 DMF solution spin-coated at 4000 r/min; spiro-MeOTAD chlorobenzene solution spin-coated at 3000 r/min; Ag evaporated.
Activation100 C anneal in glovebox; 12 h air oxidation of hole transport layer
Scalability contextArticle notes one-step solution processing is low-cost, simple, and favourable for large-scale preparation, but device fabrication here is lab-scale.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2from 40 wt% DMF precursor solution038403-2 · 2.3
LinkerMAIfrom 40 wt% DMF precursor solution038403-2 · 2.3
SolventDMFNot specified038403-2 · 2.3
OtherTiO2 gelabout 30 nm compact layer038403-2 · 2.3
Othercommercial TiO2 paste diluted with anhydrous ethanolabout 500 nm mesoporous layer · diluted 2.5 times038403-2 · 2.3
Additivespiro-MeOTAD chlorobenzene solution doped with tBP and Li-TFSINot specified038403-2 · 2.3
OtherAgabout 100 nm electrode038403-2 · 2.3
Partial recipeSource: Main

Route 2: Other

038403-5 · 3.2 · Figure 5(a,b)

Metal precursorsPbI2
Linker precursorsMAI
SolventsDMF
Atmosphereglovebox preparation implied for perovskite layer; XRD/UV samples sealed after glovebox preparation
Temperatureroom temperature; unannealed
Timeabout 30 s spin-coating
Substrate orientationmesoporous TiO2 on compact TiO2/FTO
Work-upSpin-coated; no thermal anneal before unheated XRD/UV.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2from 40 wt% DMF precursor solution038403-5 · 3.2 · Figure 5(a,b)
LinkerMAIfrom 40 wt% DMF precursor solution038403-5 · 3.2 · Figure 5(a,b)
SolventDMFresidual DMF retained after spin coating038403-5 · 3.2 · Figure 5(a,b)
Partial recipeSource: Main

Route 3: Other

038403-2 · 2.2

Metal precursorsPbI2
Linker precursorsMAI
SolventsDMF
Temperatureroom temperature
Time1
Work-upStirred to obtain 40 wt% precursor solution.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2等摩尔比038403-2 · 2.2
LinkerMAI等摩尔比038403-2 · 2.2
SolventDMF40 wt% final precursor solution038403-2 · 2.2
Partial recipeSource: Main

Route 4: Other

038403-2 · 2.3

Metal precursorsPbI2; TiO2 gel; commercial TiO2 paste
Linker precursorsMAI; spiro-MeOTAD
SolventsGBL; anhydrous ethanol; chlorobenzene
AdditivestBP; Li-TFSI
AtmosphereTiO2 calcined in air; perovskite coating/annealing in glovebox; spiro-MeOTAD oxidised in air
Temperature550 C TiO2 calcination; 60 C precursor solution; 100 C perovskite anneal
Time0.5 h compact TiO2 calcination; 0.5 h mesoporous TiO2 calcination; 1 h perovskite anneal in methods; 12 h air oxidation
Substrate orientationetched FTO glass
Oxidant / reductantair oxidation of spiro-MeOTAD
Work-upFTO etched and ultrasonically cleaned; compact and mesoporous TiO2 layers formed; heated 60 C MAPbI3 GBL solution spin-coated at 4000 r/min; spiro-MeOTAD chlorobenzene solution spin-coated at 3000 r/min; Ag evaporated.
Activation100 C anneal in glovebox; 12 h air oxidation of hole transport layer
Scalability contextOne-step solution processing is described as simple and potentially suitable for large-scale preparation.
Show 7 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2from 40 wt% GBL precursor solution038403-2 · 2.3
LinkerMAIfrom 40 wt% GBL precursor solution038403-2 · 2.3
SolventGBLNot specified038403-2 · 2.3
OtherTiO2 gelabout 30 nm compact layer038403-2 · 2.3
Othercommercial TiO2 paste diluted with anhydrous ethanolabout 500 nm mesoporous layer · diluted 2.5 times038403-2 · 2.3
Additivespiro-MeOTAD chlorobenzene solution doped with tBP and Li-TFSINot specified038403-2 · 2.3
OtherAgabout 100 nm electrode038403-2 · 2.3
Partial recipeSource: Main

Route 5: Other

038403-2 · 2.2

Metal precursorsPbI2
Linker precursorsMAI
SolventsGBL
Temperature60
Time1
Work-upHeated to 60 C and stirred to obtain 40 wt% precursor solution.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2等摩尔比038403-2 · 2.2
LinkerMAI等摩尔比038403-2 · 2.2
SolventGBL40 wt% final precursor solution038403-2 · 2.2
Partial recipeSource: Main

Route 6: Drop Cast

038403-3 · 3.1 · Figure 2

Metal precursorsPbI2
Linker precursorsMAI
SolventsDMF or GBL
Temperature100
Time0.5
Substrate orientationcopper TEM grid
Work-upPrecursor solution dropped onto copper grid, quickly spun dry, then transferred to oven.
Activation100 C heating for 0.5 h
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourcePbI2from MAPbI3 precursor solution038403-3 · 3.1 · Figure 2
LinkerMAIfrom MAPbI3 precursor solution038403-3 · 3.1 · Figure 2
SolventDMF or GBLNot specified038403-3 · 3.1 · Figure 2
Complete recipeSource: Main

Route 7: Other

038403-2 · 2.1

Linker precursorsmethylamine alcohol solution; hydroiodic acid
Solventsmethylamine alcohol solution; hydroiodic acid; anhydrous ethanol; anhydrous diethyl ether
AtmosphereN2 during reaction; vacuum oven drying
Temperatureice bath reaction; 60 C rotary evaporation; 60 C vacuum drying
Time0.5 h reaction stirring; 12 h vacuum drying
Work-upRotary evaporation until yellow-white crystals form; add small amount of anhydrous ethanol if needed; wash/filter with excess anhydrous diethyl ether until white.
Activation60 C vacuum oven for 12 h
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Linker甲胺醇溶液15 mL; 0.078 mol · 27%038403-2 · 2.1
Acid氢碘酸12.5 mL; 0.066 mol · 45%038403-2 · 2.1
Solvent无水乙醇少量038403-2 · 2.1
Solvent无水乙醚大量038403-2 · 2.1