Jena S, et al. Applied Surface Science, 2021, 542, 148756.
Cetrimide bromide (CTAB) can be used to prepare antimony and tin-antimony alloy nanorods (Sb-SnSb NRs) from nanoparticle precursors (Sb-SnSb NPs) via microwave-hydrothermal method. The synergistic effect of CTAB and microwave-hydrothermal environment forces the nanoparticles to self-assemble and fuse into stacked nanorods.
The specific method is as follows:
Step I: Synthesis of Sb-SnSb Nanoparticles
Initially, 150 mmol of sodium citrate was dissolved in 180 ml of deionized water. To this solution, 50 mmol of SbCl3 and 25 mmol of SnCl2·2H2O were added and stirred until fully dissolved. The solution was then cooled to 5 °C using an ice bath containing NaCl. Once the desired temperature was reached, a separately prepared solution containing 40 mmol of NaOH and 37.5 mmol of NaBH4 in deionized water was rapidly injected into the precursor solution. This injection caused vigorous effervescence, and the solution color changed to black, indicating the formation of the nanoparticles. The reaction mixture was then allowed to warm to room temperature and stirred for 1 hour. The resulting crystalline alloy powder was collected by centrifugation, thoroughly washed with deionized water to remove any unreacted residues, and finally rinsed with acetone before being dried in a vacuum oven.
Step II: Synthesis of Sb-SnSb Nanorods
First, 42.86 mg of CTAB, corresponding to its critical micelle concentration at room temperature, was dissolved in 120 ml of deionized water. The nanoparticle mixture (50 mg) was then added to the CTAB solution and ultrasonicated for 1 hour, resulting in a black colloidal solution, indicating uniform dispersion of the nanoparticles. Next, 40 ml of this colloidal solution was transferred into a Teflon-lined autoclave, which was then sealed and placed in a microwave-hydrothermal reactor. The autoclave was exposed to microwave irradiation pulses of 700 W, maintaining an isothermal condition of 120 °C for 90 minutes. After the reaction, the autoclave was cooled to room temperature, and the crystalline powder was retrieved via centrifugation. The powder was then washed sequentially with water and acetone before drying in a vacuum oven.