Synthesis evidence

High-performance field-effect transistor glucose biosensors based on bimetallic Ni/Cu metal-organic frameworks

Wang B., Luo Y., Gao L. et al. · Biosensors and Bioelectronics · 2021 · 112736

12 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

2 · 2.3

Metal precursorspreformed GOD-GA-Ni/Cu-MOFs (7:1)-FET
Solventsnot specified for BSA blocking solution beyond BSA concentration
Additivesbovine serum albumin
Atmosphererefrigerated
Temperature4 degC
Time12 h
Substrate orientationliquid cell of FET device
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
AdditiveBSA5 uL · 1 wt%2 · 2.3
Complete recipeSource: SI

Route 2: Hydrothermal

S1

Metal precursorsCuSO4.5H2O
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 wafer (SiO2 285 +/- 10 nm, p-type doped), 2.5 x 2 cm2 chip; ultraviolet lithography/lift-off defined 50 um x 1000 um channel; Ti 10 nm/Au 100 nm source-drain electrodes by magnetron sputtering. Cleaned FET suspended upside down on reaction solution surface.
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceCuSO4.5H2O7.0 mg (0.028 mmol)S1
LinkerHATP.6HCl10.0 mg (0.019 mmol)S1
Solventdeionized water5 mL in each of two beakersS1
BaseNH3.H2O0.3 mLS1
Partial recipeSource: Main

Route 3: Other

2 · 2.3

Metal precursorspreformed Ni/Cu-MOFs (7:1)-FET
Linker precursorsglutaraldehyde
SolventsPBS solution
Additivesglutaraldehyde
Atmosphereambient
Temperatureroom temperature
Time1 h GA; 5-10 min drying inferred from sensor workup
Substrate orientationliquid cell of FET device
Work-uprinsed with PBS several times
Show 1 structured reagent record
RoleReagentAmount / concentrationSource
Additiveglutaraldehyde (GA)5 uL · 0.25% in PBS2 · 2.3
Complete recipeSource: Main

Route 4: Other

2 · 2.3

Metal precursorspreformed Ni-MOFs-FET
Linker precursorsglutaraldehyde
SolventsPBS solution
Additivesglucose oxidase; glutaraldehyde
Atmosphereambient and refrigerated
Temperatureroom temperature for GA; 4 degC for GOD
Time1 h GA; overnight GOD
Substrate orientationliquid cell of FET device
Work-uprinsed with PBS several times
Show 2 structured reagent records
RoleReagentAmount / concentrationSource
Additiveglucose oxidase (GOD)5 uL · 1.0 mg/mL in PBS2 · 2.3
Additiveglutaraldehyde (GA)5 uL · 0.25% in PBS2 · 2.3
Complete recipeSource: Main

Route 5: Other

2 · 2.3 · Fig. 1b

Metal precursorspreformed Ni/Cu-MOFs (7:1)-FET
Linker precursorsglutaraldehyde linker between GOD and MOF surface
SolventsPBS solution
Additivesglucose oxidase; glutaraldehyde
Atmosphereambient for GA incubation; refrigerator for GOD incubation
Temperatureroom temperature for GA; 4 degC for GOD
Time1 h GA; overnight GOD; 5-10 min drying
Substrate orientationliquid cell of FET device
Work-uprinsed with PBS several times after GA and after GOD; dried at room temperature
Show 3 structured reagent records
RoleReagentAmount / concentrationSource
Additiveglucose oxidase (GOD)5 uL · 1.0 mg/mL in PBS2 · 2.3 · Fig. 1b
Additiveglutaraldehyde (GA)5 uL · 0.25% in PBS2 · 2.3 · Fig. 1b
SolventPBS solutionNot specified2 · 2.3 · Fig. 1b
Partial recipeSource: SI

Route 6: Hydrothermal

S1

Metal precursorsNi source not fully specified in supplied article/SI; prepared according to Wang et al. 2019 prior work
Linker precursorsHATP.6HCl inferred from material family
Solventsnot fully reported
Additivesnot fully reported
Atmospherenot reported
Time1
Substrate orientationSi/SiO2 wafer (SiO2 285 +/- 10 nm, p-type doped), 2.5 x 2 cm2 chip; ultraviolet lithography/lift-off defined 50 um x 1000 um channel; Ti 10 nm/Au 100 nm source-drain electrodes by magnetron sputtering.
Work-upFET chip fabrication, rinsing and drying are reported in SI S1; Ni-MOF growth recipe itself is referred to prior work.
ActivationFET chip dried at 100 degC for 2 h before MOF growth
Partial recipeSource: Both

Route 7: Hydrothermal

2 · 2.2

Metal precursorsNiCl2.6H2O and CuSO4.5H2O with feeding Ni:Cu 10:1
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 Ti/Au FET device suspended upside down on reaction solution surface
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2Oadjusted to feeding Ni:Cu 10:1; exact mass not reported2 · 2.2
Metal SourceCuSO4.5H2Oadjusted to feeding Ni:Cu 10:1; exact mass not reported2 · 2.2
LinkerHATP.6HCl10.0 mg (amount reported for 7:1 route; variant amount not separately reported)2 · 2.2
BaseNH3.H2O0.3 mL (reported for 7:1/Cu route; variant amount not separately reported)2 · 2.2
Partial recipeSource: Both

Route 8: Hydrothermal

2 · 2.2

Metal precursorsNiCl2.6H2O and CuSO4.5H2O with feeding Ni:Cu 1:1
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 Ti/Au FET device suspended upside down on reaction solution surface
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2Oadjusted to feeding Ni:Cu 1:1; exact mass not reported2 · 2.2
Metal SourceCuSO4.5H2Oadjusted to feeding Ni:Cu 1:1; exact mass not reported2 · 2.2
LinkerHATP.6HCl10.0 mg (amount reported for 7:1 route; variant amount not separately reported)2 · 2.2
BaseNH3.H2O0.3 mL (reported for 7:1/Cu route; variant amount not separately reported)2 · 2.2
Partial recipeSource: Both

Route 9: Hydrothermal

2 · 2.2

Metal precursorsNiCl2.6H2O and CuSO4.5H2O with feeding Ni:Cu 1:7
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 Ti/Au FET device suspended upside down on reaction solution surface
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2Oadjusted to feeding Ni:Cu 1:7; exact mass not reported2 · 2.2
Metal SourceCuSO4.5H2Oadjusted to feeding Ni:Cu 1:7; exact mass not reported2 · 2.2
LinkerHATP.6HCl10.0 mg (amount reported for 7:1 route; variant amount not separately reported)2 · 2.2
BaseNH3.H2O0.3 mL (reported for 7:1/Cu route; variant amount not separately reported)2 · 2.2
Partial recipeSource: Both

Route 10: Hydrothermal

2 · 2.2

Metal precursorsNiCl2.6H2O and CuSO4.5H2O with feeding Ni:Cu 20:1
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 Ti/Au FET device suspended upside down on reaction solution surface
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2Oadjusted to feeding Ni:Cu 20:1; exact mass not reported2 · 2.2
Metal SourceCuSO4.5H2Oadjusted to feeding Ni:Cu 20:1; exact mass not reported2 · 2.2
LinkerHATP.6HCl10.0 mg (amount reported for 7:1 route; variant amount not separately reported)2 · 2.2
BaseNH3.H2O0.3 mL (reported for 7:1/Cu route; variant amount not separately reported)2 · 2.2
Partial recipeSource: Both

Route 11: Hydrothermal

2 · 2.2

Metal precursorsNiCl2.6H2O and CuSO4.5H2O with feeding Ni:Cu 30:1
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 Ti/Au FET device suspended upside down on reaction solution surface
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Show 4 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2Oadjusted to feeding Ni:Cu 30:1; exact mass not reported2 · 2.2
Metal SourceCuSO4.5H2Oadjusted to feeding Ni:Cu 30:1; exact mass not reported2 · 2.2
LinkerHATP.6HCl10.0 mg (amount reported for 7:1 route; variant amount not separately reported)2 · 2.2
BaseNH3.H2O0.3 mL (reported for 7:1/Cu route; variant amount not separately reported)2 · 2.2
Complete recipeSource: Both

Route 12: Hydrothermal

2 · 2.2 · Fig. 1

Metal precursorsNiCl2.6H2O and CuSO4.5H2O, feeding Ni:Cu 7:1
Linker precursorsHATP.6HCl
Solventsdeionised water
AdditivesNH3.H2O
Atmospherenot reported
Temperature65
Time1
Substrate orientationSi/SiO2 wafer (SiO2 285 +/- 10 nm, p-type doped), 2.5 x 2 cm2 chip; ultraviolet lithography/lift-off defined 50 um x 1000 um channel; Ti 10 nm/Au 100 nm source-drain electrodes by magnetron sputtering. Cleaned FET suspended upside down on reaction solution surface.
Work-upFET device UV-ozone cleaned for about 30-60 min, suspended upside down on reaction solution, heated in water bath at 65 degC for 60 min, cooled to room temperature, rinsed with deionized water and ethanol several times, then dried in vacuum oven at 100 degC for 120 min; silicon rubber used to form liquid cell.
Activationvacuum oven drying at 100 degC for 120 min
Scalability contextAuthors state large, uniform films were grown in situ on pre-prepared FET devices.
Show 5 structured reagent records
RoleReagentAmount / concentrationSource
Metal SourceNiCl2.6H2O6.6 g (0.028 mmol; source text likely has unit inconsistency)2 · 2.2 · Fig. 1
Metal SourceCuSO4.5H2O1.0 g (0.004 mmol; source text likely has unit inconsistency)2 · 2.2 · Fig. 1
Solventdeionized water5 mL for metal solution; 5 mL for ligand solution2 · 2.2 · Fig. 1
BaseNH3.H2O0.3 mL2 · 2.2 · Fig. 1
LinkerHATP.6HCl10.0 mg (0.028 mmol)2 · 2.2 · Fig. 1