Preparation method of Fe3O4 nanoparticles with cluster structure
A technology of ferric tetroxide and nanoparticles, which is applied in the directions of preparations, pharmaceutical formulations, and emulsion delivery for in vivo experiments, can solve the problems of dual-modal MRI diagnosis without ferric tetroxide nanoparticles, and achieve MR. The effect of imaging signal enhancement
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Embodiment 1
[0040] (1) Dissolve 0.65g of anhydrous ferric chloride in 40mL of diethylene glycol (also known as diethylene glycol, DEG), add 0.47g of sodium citrate (Na 3 Cit), stirred at 80°C for 1 h in an air atmosphere, and then added 1.312 g of anhydrous sodium acetate powder after the sodium citrate was completely dissolved, and continued to stir until the sodium acetate powder was completely dissolved, then transferred the solution to a 50 mL autoclave, and React at 200°C for 4 hours; after the reaction, naturally cool to room temperature, transfer the product to a 50mL centrifuge tube and centrifuge at 8500rpm for 15 minutes, discard the supernatant, redissolve with absolute ethanol, centrifuge at 8500rpm for 15 minutes, repeat the operation 3 times, The precipitate was then dried at 60°C to obtain ultra-small Fe 3 o 4 Nanoparticles, ultra-small iron oxide nanoparticles with sodium citrate stabilized surfaces.
[0041] (2) Ultra-small Fe in step (1) 3 o 4Nanoparticles (30mg) wer...
Embodiment 2
[0044] Get ultra-small Fe in embodiment 1 respectively 3 o 4 Fe nanoparticles and clusters 3 o 4 / 2 mg of Cystamine nanoparticles were dissolved in 2 mL of ultrapure water to obtain a nanoparticle suspension, which was uniformly ultrasonicated, and the surface potential and hydrated particle size were measured. The test results are shown in Table 1. The test results show that: the prepared ultra-small Fe 3 o 4 Fe nanoparticles and clusters 3 o 4 The surface potentials of / Cystamine nanoparticles were -33.2 and -21.4mV respectively; the hydrated particle diameters were 25.6 and 134.4nm. From the experimental results, the surface potential of monodisperse ultra-small iron oxide nanoparticles increases after cross-linking into clusters, and the hydrodynamic diameter increases significantly. Changes in surface potential and hydrated particle size indicate cluster Fe 3 o 4 / Cystamine nanoparticles have been formed.
[0045] Table 1
[0046] sample
Embodiment 3
[0048] Get ultra-small Fe in embodiment 1 respectively 3 o 4 Fe nanoparticles and clusters 3 o 4 / Cystamine nanoparticles 5mg carry out infrared spectrum test (such as figure 1 shown) and thermogravimetric analysis (as figure 2 shown). By analyzing the infrared spectrum (such as figure 1 ), 466-601cm -1 The characteristic absorption peaks appearing on the Fe 3 o 4 Stretching vibration of upper Fe-O, 3451cm -1 The nearby peak is the stretching vibration peak of OH on the water molecule, 2931cm -1 and 2800cm -1 The nearby characteristic absorption peak is attributed to the stretching vibration of methylene in sodium citrate. At the same time at 1396-1642cm -1 It is the stretching vibration of C=O. And the strong absorption peak of 1736 in the curve b belongs to the amino group and Fe of cystamine dihydrochloride 3 o 4 An amide bond formed by binding carboxyl groups on the surface. 551cm -1 The characteristic peak at the position is obviously enhanced, which s...
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