Synthesis evidence

Utilization of counter anions for charge transportation in the electrical device fabrication of Zn(ii) metal-organic frameworks

Das K.S., Pal B., Saha S. et al. · Dalton Transactions · 2020 · 17005-17016

5 structured synthesis routes

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

Complete recipeSource: Main

Route 1: Other

17006 · Synthesis of {[Zn(H2MBP)1.5](BF4)}n (1)

Metal precursorsZn(BF4)2.xH2O
Linker precursorsH2MBP
Solventsmethanol; distilled water; water-methanol (1:1) wash
Atmospherenot specified; beaker covered with paraffin tape
Temperatureroom temperature
Time168
Work-upmetal methanolic solution added dropwise to ligand solution; water added until precipitate dissolved; filtered; covered with paraffin tape for 7 days; crystals washed with water-methanol (1:1) and dried in air
Activationdried in air
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH2MBP148 mg, 1.0 mmol17006 · Synthesis of {[Zn(H2MBP)1.5](BF4)}n (1)
Metal SourceZn(BF4)2.xH2O239 mg, 1.0 mmol17006 · Synthesis of {[Zn(H2MBP)1.5](BF4)}n (1)
Solventmethanolmethanolic solutions17006 · Synthesis of {[Zn(H2MBP)1.5](BF4)}n (1)
Solventdistilled water10 mL17006 · Synthesis of {[Zn(H2MBP)1.5](BF4)}n (1)
Solventwater-methanol (1:1)wash17006 · Synthesis of {[Zn(H2MBP)1.5](BF4)}n (1)
Partial recipeSource: Main

Route 2: Other

17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1

SolventsN,N-dimethylformamide (DMF)
AtmosphereAl deposition under 10^-6 Torr; drying atmosphere hot air
Temperaturehot air oven; exact drying temperature not reported
Substrate orientationfront side of properly cleaned ITO-coated glass
Work-uphomogeneous DMF solution prepared by ultrasonication; spin-coated at 1000 rpm; film dried in hot air oven; Al deposited by HINDHIVAC vacuum coating
Activationdevice annealed in vacuum oven at 70 C for several minutes before I-V measurement
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 1Not specified17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
SolventN,N-dimethylformamide (DMF)Not specified17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
OtherITO-coated glass substrateNot specified17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
OtherAl metal top contactaround 1 um thickness17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
Partial recipeSource: Main

Route 3: Other

17006 · Synthesis of {[Zn3(H2MBP)4(H2O)4(SO4)3](H2O)7}n (2)

Metal precursorsZnSO4.7H2O
Linker precursorsH2MBP
Solventsmethanol; distilled water; water-methanol (1:1) wash inferred from same route as compound 1
Atmospherenot specified; route stated as similar to compound 1
Temperaturemild heating after addition of water; exact temperature not reported
Time168 inferred from similar preparation to compound 1
Work-upsimilar to compound 1, using ZnSO4.7H2O instead of Zn(BF4)2.xH2O; mild heating after adding water to dissolve precipitate; white block-shaped crystals obtained
Activationnot explicitly repeated; likely dried in air by similarity to compound 1
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerH2MBP148 mg, 1.0 mmol inferred from compound 117006 · Synthesis of {[Zn3(H2MBP)4(H2O)4(SO4)3](H2O)7}n (2)
Metal SourceZnSO4.7H2O287.56 mg, 1.0 mmol17006 · Synthesis of {[Zn3(H2MBP)4(H2O)4(SO4)3](H2O)7}n (2)
Solventmethanolmethanolic solutions inferred from compound 117006 · Synthesis of {[Zn3(H2MBP)4(H2O)4(SO4)3](H2O)7}n (2)
Solventdistilled water10 mL inferred from compound 117006 · Synthesis of {[Zn3(H2MBP)4(H2O)4(SO4)3](H2O)7}n (2)
Partial recipeSource: Main

Route 4: Other

17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1

SolventsN,N-dimethylformamide (DMF)
AtmosphereAl deposition under 10^-6 Torr; drying atmosphere hot air
Temperaturehot air oven; exact drying temperature not reported
Substrate orientationfront side of properly cleaned ITO-coated glass
Work-uphomogeneous DMF solution prepared by ultrasonication; spin-coated at 1000 rpm; film dried in hot air oven; Al deposited by HINDHIVAC vacuum coating
Activationdevice annealed in vacuum oven at 70 C for several minutes before I-V measurement
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercompound 2Not specified17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
SolventN,N-dimethylformamide (DMF)Not specified17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
OtherITO-coated glass substrateNot specified17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
OtherAl metal top contactaround 1 um thickness17006 · Fabrication of ITO/synthesized zinc-based MOF/Al-based Schottky barrier diodes · Fig. 1
Complete recipeSource: SI

Route 5: Other

p002 · Synthesis and Characterization of H2MBP

Linker precursorspyrazole
Solventshot water for dissolution; absolute ethanol for recrystallisation
Additivesdilute aqueous NaOH solution
Atmosphereair oven
Temperature200
Time2
Work-upcooled slowly to room temperature; dissolved in hot water; neutralised dropwise with dilute aqueous NaOH with stirring; precipitate filtered and washed several times with distilled water; dried at room temperature; recrystallised from absolute ethanol
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Linkerpyrazole3.2 gp002 · Synthesis and Characterization of H2MBP
Otherdibromomethane1.6 mlp002 · Synthesis and Characterization of H2MBP
Basedilute aqueous NaOH solutiondropwise additionp002 · Synthesis and Characterization of H2MBP
Solventdistilled waterseveral washesp002 · Synthesis and Characterization of H2MBP
Solventabsolute ethanolNot specifiedp002 · Synthesis and Characterization of H2MBP