Method Article
Protocol for synthesis of DADS-nFeS
Lizeng Gao
Gao Lab (Yangzhou University)
Corresponding Author
Abstract
This protocol describes the detailed procedure for preparation of DADS-nFeS. To get our target nanoparticle with stable property, we synthesised DADS-nFeS by solvothermal method with high temperatures and pressures.
Keywords
Iron oxide, nanoparticles, diallyl sulfide, solvothermal
Figures
Figure 1
Introduction
This protocol describes the detailed procedure for preparation of DADS-nFeS. We synthesized DADS-nFeS by solvothermal method under high temperature and pressure in a sealed autoclave reactor.
Reagents
ethylene glycol, FeCl3•6H2O, sodium acetate(NaOAc), diallyl sulfide(DADS)
Equipment
magnetic stirring bar, oven, Teflon-lined stainless steel autoclave
Procedure
- 0.82 g FeCl3•6H2O was dissolved uniformly in 40 mL ethylene glycol in a beaker.
- Keep stirring the mixture with a stir bar till it turned orange without distinct precipitation. CAUTION If the reactants added into the ethylene glycol cannot be dispersed easily, ultrasonic treatment on the mixture for 10 min or even longer would help.
- 3.6 g Sodium acetate was added into the mixture until the iron source was totally dissolved and the suspension became dark brown.
- Appropriate amount of diallyl sulfide was added into the mixture during the mixing process respectively. CAUTION Owing to the pungent smell of DADS, the whole process was performed in the fume cupboard and the beaker dissolved with mixed solution need to be covered by plastic wrap.
- The mixture was transferred into a 50 mL Teflon-lined stainless steel autoclave in the fume cupboard after being sufficiently stirred and sonicated. CAUTION The screws of the stainless steel autoclave should be tightened for guaranteed pressure and safety.
- The reaction was conducted at 200℃ in an oven for 12 h.
- After the reaction was finished, the Teflon-lined stainless steel autoclave was cooled to room temperature.
- The product in the Teflon-lined stainless steel autoclave was poured into a 50 ml centrifuge tube with the supernatant discarded.
- The product was dissolved in ethanol and washed for several times through centrifugal separation at 5000 g for 5 min until the washings became clear.
- The product of DADS-nFeS was obtained after drying at 60℃ for 4 h and preserved at 4℃
Timing
14 h or longer (including the mixing process and the reaction time under high temperature and high pressure)
Anticipated Results
The new formed products are black (or brown if the drying process is much more sufficent) powder which consist of hexagonal sheet-like nanostructures and sphere nanoparticles under the electron microscope.
References
1.Gao, L. et al. Intrinsic peroxidase-like activity of ferromagnetic nanoparticles. Nat Nanotechnol 2, 577-583(2007).
2.Gao, L. Z. et al. Magnetite Nanoparticle-Linked Immunosorbent Assay. J Phys Chem C 112, 17357-17361(2008).
3.Fan, K. et al. Optimization of Fe3O4 nanozyme activity via single amino acid modification mimicking an enzyme active site.Chem Commun 53, 424-427(2016).
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Posted 03 Dec, 2018
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Subject Areas
Nanoscience and technology
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Method Article
Protocol for synthesis of DADS-nFeS
Lizeng Gao
Gao Lab (Yangzhou University)
Corresponding Author
Article
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Abstract
This protocol describes the detailed procedure for preparation of DADS-nFeS. To get our target nanoparticle with stable property, we synthesised DADS-nFeS by solvothermal method with high temperatures and pressures.
Figures
Figure 1
Introduction
This protocol describes the detailed procedure for preparation of DADS-nFeS. We synthesized DADS-nFeS by solvothermal method under high temperature and pressure in a sealed autoclave reactor.
Reagents
ethylene glycol, FeCl3•6H2O, sodium acetate(NaOAc), diallyl sulfide(DADS)
Equipment
magnetic stirring bar, oven, Teflon-lined stainless steel autoclave
Procedure
- 0.82 g FeCl3•6H2O was dissolved uniformly in 40 mL ethylene glycol in a beaker.
- Keep stirring the mixture with a stir bar till it turned orange without distinct precipitation. CAUTION If the reactants added into the ethylene glycol cannot be dispersed easily, ultrasonic treatment on the mixture for 10 min or even longer would help.
- 3.6 g Sodium acetate was added into the mixture until the iron source was totally dissolved and the suspension became dark brown.
- Appropriate amount of diallyl sulfide was added into the mixture during the mixing process respectively. CAUTION Owing to the pungent smell of DADS, the whole process was performed in the fume cupboard and the beaker dissolved with mixed solution need to be covered by plastic wrap.
- The mixture was transferred into a 50 mL Teflon-lined stainless steel autoclave in the fume cupboard after being sufficiently stirred and sonicated. CAUTION The screws of the stainless steel autoclave should be tightened for guaranteed pressure and safety.
- The reaction was conducted at 200℃ in an oven for 12 h.
- After the reaction was finished, the Teflon-lined stainless steel autoclave was cooled to room temperature.
- The product in the Teflon-lined stainless steel autoclave was poured into a 50 ml centrifuge tube with the supernatant discarded.
- The product was dissolved in ethanol and washed for several times through centrifugal separation at 5000 g for 5 min until the washings became clear.
- The product of DADS-nFeS was obtained after drying at 60℃ for 4 h and preserved at 4℃
Timing
14 h or longer (including the mixing process and the reaction time under high temperature and high pressure)
Anticipated Results
The new formed products are black (or brown if the drying process is much more sufficent) powder which consist of hexagonal sheet-like nanostructures and sphere nanoparticles under the electron microscope.
References
1.Gao, L. et al. Intrinsic peroxidase-like activity of ferromagnetic nanoparticles. Nat Nanotechnol 2, 577-583(2007).
2.Gao, L. Z. et al. Magnetite Nanoparticle-Linked Immunosorbent Assay. J Phys Chem C 112, 17357-17361(2008).
3.Fan, K. et al. Optimization of Fe3O4 nanozyme activity via single amino acid modification mimicking an enzyme active site.Chem Commun 53, 424-427(2016).
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