Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures†

doi:10.7503/cjcu20140669

Abstract

Abstract:

3D flower-like α-FeOOH nanoparticles were synthesized by means of mild-temperature reflux method, and the samples were characterized via X-ray diffraction(XRD) and scanning electron microscopy(SEM). The influencing factors such as the reaction time, the reaction temperature, the concentration of urea, and the amount of ethanol were systematically investigated. The adsorption capacity of the α-FeOOH nanoparticles for diclofenac sodium was also tested. The results show that the sample prepared with 0.1 mol/L urea and 20%(volume fraction) ethanol at 90 ℃ for 6 h is in high structural uniformity with good crystal quality and has the best adsorption capactity of 199.2 mg/g for diclofenac sodium. The formation mechanism of the flower-like α-FeOOH nanostructures is involved with a combination of oriented attachment and epitaxial overgrowth. The fresh nanonuclei are formed in solution at the early reaction stage with high surface energy, then aggregate together to minimize the interfacial energy. The olive-like agglomerates orient into short clusters, continue to grow along z axis till the complete flower-like structures are formed.

Key words: 3D flower-like structure, α-FeOOH, -FeOOH, Low-temperature reflux, Diclofenac sodium, Adsorption property

CLC Number:

O614

TrendMD:

XU Junge, LI Yunqin, YUAN Baoling, CUI Haojie, FU Minglai. Synthesis and Characterization of 3D Flower-like α-FeOOH Nanostructures^†[J]. Chem. J. Chinese Universities, 2015, 36(1): 48.

Figures/Tables 9

Fig.1 SEM images of the samples obtained at 0.5 h(A), 1 h(B), 2 h(C), 4 h(D), 6 h(E) and 8 h(F)

Fig.2 XRD patterns of the intermediate products obtained at 0.5(a), 1(b), 2(c), 4(d), 6(e) and 8(f)

Scheme 1 Schematic illustrations for the formation process of the flower-like α-FeOOH nanostructures

Fig.3 SEM images of the samples obtained at 70 ℃(A), 80 ℃(B) and 100 ℃(C)

Fig.4 XRD patterns of the samples obtained at 70 ℃(a), 80 ℃(b), 90 ℃(c) and 100 ℃(d)

Fig.5 SEM images of the samples obtained at different concentrations of urea c(urea)/(mol·L-1): (A) 0.05; (B) 0.2.

Fig.6 SEM images of the samples obtained with different amount of ethanol Volume fraction of ethanol: (A) 0; (B) 10%; (C) 40%.

Fig.7 N2 adsorption and desorption isotherms(A) and pore-size distribution(B) of the typical sample

Fig.8 Adsorption isotherms of diclofenac sodium using different samples a. c(urea): 0.1 mol/L, volume fraction of ethanol: 20%, 90 ℃, 6 h; b. c(urea): 0.1 mol/L, volume fraction of ethanol: 20%, 80 ℃, 6 h; c. c(urea): 0.1 mol/L, volume fraction of ethanol: 40%, 90 ℃, 6 h; d. c(urea): 0.1 mol/L, volume fraction of ethanol: 20%, 90 ℃, 2 h.

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