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         A mixture of Ni(acac) 2 (0.77g, 3.0 mmol) and TOP (4.0 mL, 9.0 mmol) in oleylamine (20mL) was slowly heated from room temperature to 493 K for 15 min under an inert atmosphere and was allowed to stir at 493 K for 45 min. After the reaction, the resulting black mixture was cooled at room temperature, and the particles were precipitated by adding ethanol (40 mL) and centrifuging at 10000 rpm for 20 min. Finally, the nickel nanoparticles were dispersed in cyclohexane.
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Cyclohexane (25 mL) was added into a mixture of igepal CO-630 (8.0 mL) and NH4OH aqueous solution (1.0 mL) and stirred for 10 min. The nickel particle dispersion in cyclohexane (25 mL, 60 mM with respect to the nickel precursor concentration) was added into the mixture and allowed to stir rapidly for 30 s. TMOS (1.0 mL) and C18TMS (1.0 mL) were added, and the mixture was stirred for 1 h at room temperature. The resulting Ni@SiO2 core -shell particles were precipitated by adding methanThe ethanol dispersion (30 mL) of the Ni@SiO2 core -shell particles (50 mM with respect to the nickel precursor concentration) was treated with hydrochloric acidol (10 mL), washed with ethanol thoroughly, and redispersed in ethanol. The ethanol dispersion (30 mL) of the Ni@SiO2 core -shell particles (50 mM with respect to the nickel precursor concentration) was treated with hydrochloric acid (10 mL, 0.45 M) at room temperature for 30 min. The product was collected by centrifugation at 10 000 rpm for 30 min and washed with ethanol thoroughly. After drying at room temperature, the powders were placed in the ceramic boat in a glass tube oven, heated at a ramping rate of 4 K/min to 773K, and calcined at 773 K for 2 h under a hydrogen flow of 200 cc/min. After calcination, the resulting powders were cooled to room tem-perature and immediately submerged into anhydrous ethanol (20 mL) under a hydrogen environment in order to prevent surface oxidation of the nickel cores.
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