Synthesis evidence

A highly oriented conductive MOF thin film-based Schottky diode for self-powered light and gas detection

Cao L.-A., Yao M.-S., Jiang H.-J. et al. · Journal of Materials Chemistry A · 2020 · 9085-9090

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

p005 / article p.9089 · Experimental - Preparation of Ag/EC-MOFs/n-Si/Al photodetector and gas sensing devices · Fig. 3a

Metal precursorsAg electrode and Al electrode by thermal evaporation
Linker precursorsEC-MOF interlayer supplied by air/liquid interface or LBL liquid-phase epitaxial spray method
Solventsethanol for removing EC-MOF outside electrode area
Atmospherenot specified for thermal evaporation
Substrate orientationcommercial n-type Si (100) wafer
Work-upEC-MOF outside the electrode area removed by an ethanol-dipped cotton swab.
Scalability contextAg top electrode area 0.5 mm x 0.5 mm; semitransparent Ag thickness ~20 nm; Al back electrode about 50 nm.
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Othercommercial n-type Si (100) waferNot specifiedp005 / article p.9089 · Experimental - Preparation of Ag/EC-MOFs/n-Si/Al photodetector and gas sensing devices · Fig. 3a
OtherAg electrode0.5 mm x 0.5 mm; ~20 nm thickp005 / article p.9089 · Experimental - Preparation of Ag/EC-MOFs/n-Si/Al photodetector and gas sensing devices · Fig. 3a
OtherAl electrodeabout 50 nmp005 / article p.9089 · Experimental - Preparation of Ag/EC-MOFs/n-Si/Al photodetector and gas sensing devices · Fig. 3a
Solventethanolethanol-dipped cotton swabp005 / article p.9089 · Experimental - Preparation of Ag/EC-MOFs/n-Si/Al photodetector and gas sensing devices · Fig. 3a
Complete recipeSource: Main

Route 2: Other

p005 / article p.9089 · Experimental - Preparation of the Cu3(C18H6O6)2 thin film

Metal precursorsCu(OAc)2.H2O in ethanol, 0.1 mM (same as Cu3(C18H6(NH)6)2 route)
Linker precursorsHHTP ligand; concentration not restated but same process as Cu3(C18H6(NH)6)2 route except ligand
Solventsethanol
Additivesno ammonium hydroxide
Atmosphereroom temperature; dried by N2 after rinse steps in the analogous route
Temperatureroom temperature
Substrate orientationfunctionalised n-Si substrate in device context
Work-upAnalogous ethanol rinse/N2 drying inferred from stated same process as Cu3(C18H6(NH)6)2, except ligand and base.
Scalability context20 nm film obtained after ten deposition cycles.
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2.H2O in ethanol0.1 mMp005 / article p.9089 · Experimental - Preparation of the Cu3(C18H6O6)2 thin film
LinkerHHTPnot restatedp005 / article p.9089 · Experimental - Preparation of the Cu3(C18H6O6)2 thin film
SolventethanolNot specifiedp005 / article p.9089 · Experimental - Preparation of the Cu3(C18H6O6)2 thin film
Complete recipeSource: Main

Route 3: Other

p005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 thin films

Metal precursorsCu(OAc)2.H2O in ethanol, 0.1 mM
Linker precursorsHITP ligand in ethanol, 0.01 mM
Solventsethanol; DI water, acetone, ethanol for substrate washing
Additivesammonium hydroxide (28%) to regulate HITP solution pH to 8.5
Atmosphereroom temperature; dried by N2 after rinse steps
Temperatureroom temperature
Substrate orientationfunctionalised n-Si substrates; Si substrates first washed and piranha-treated to functionalise surface -OH
Work-upBetween sprays, films were rinsed by spraying pure ethanol for 20 s to remove unreacted reactants, then dried by N2.
Scalability contextThickness controlled by deposition cycles; 20-100 nm films fabricated.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCu(OAc)2.H2O in ethanol0.1 mMp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 thin films
LinkerHITP ligand in ethanol0.01 mMp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 thin films
SolventethanolNot specifiedp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 thin films
Baseammonium hydroxide (28%)to pH 8.5 · 28%p005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 thin films
AcidPiranha solution H2SO4 (95-98%) : H2O2 (30%) = 7 : 3substrate immersion at 100 C for 1 hp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 thin films
Complete recipeSource: Main

Route 4: Other

p005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 powders

Metal precursorsCuSO4.5H2O, 7 mg (0.028 mmol)
Linker precursorsHITP ligand, 10 mg (0.019 mmol)
SolventsDI water, 2 mL for copper/base solution and 2 mL for HITP solution; ethanol for washing
AdditivesNH3.H2O, 75 uL
Atmosphereroom temperature; vacuum drying
Temperatureroom temperature; drying at 60
Time3 h stirring; 12 h vacuum drying
Work-upProducts collected from reactor and washed three times with DI water and ethanol respectively.
ActivationDried in vacuum at 60 C for 12 h
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O7 mg (0.028 mmol)p005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 powders
BaseNH3.H2O75 uLp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 powders
LinkerHITP ligand10 mg (0.019 mmol)p005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 powders
SolventDI water2 mL + 2 mLp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 powders
Solventethanolwashing solventp005 / article p.9089 · Experimental - Preparation of Cu3(C18H6(NH)6)2 powders
Partial recipeSource: Main

Route 5: Air Liquid Interface

p005 / article p.9089 · Experimental - Preparation of Ni3(C18H6(NH)6)2 thin films

Metal precursorsnickel chloride hexahydrate (NiCl2.6H2O), 6.6 mg (0.028 mmol)
Linker precursorsHITP, 10.0 mg (0.019 mmol)
SolventsDI water, 20.0 mL
Additivesammonium hydroxide, 0.3 mL
Atmospherenot specified
Temperature65
Time~0.025
Substrate orientationair/liquid interface; substrate not specified in main text
Work-upnot specified in main text
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
LinkerHITP10.0 mg (0.019 mmol)p005 / article p.9089 · Experimental - Preparation of Ni3(C18H6(NH)6)2 thin films
Metal Sourcenickel chloride hexahydrate (NiCl2.6H2O)6.6 mg (0.028 mmol)p005 / article p.9089 · Experimental - Preparation of Ni3(C18H6(NH)6)2 thin films
SolventDI water20.0 mLp005 / article p.9089 · Experimental - Preparation of Ni3(C18H6(NH)6)2 thin films
Baseammonium hydroxide0.3 mLp005 / article p.9089 · Experimental - Preparation of Ni3(C18H6(NH)6)2 thin films