Controllable Synthesis of γ-Al2O3 Hexagonal Nanoplates with Ionic Liquids as the Template†

doi:10.7503/cjcu20180300

Abstract

Abstract:

γ-Al₂O₃ hexagonal nanoplates with unique crystal orientations were synthesized via an ionic liquid-assisted hydrothermal method using aluminum chloride as the aluminum source, n-butylamine as the precipitant and [Bmim]BF₄ as the template. The synthesized products were characterized by means of X-ray diffraction(XRD), scanning electron microscopy(SEM), transmission electron microscopy(TEM), Fourier transform infrared spectroscopy(FTIR) and N₂ isothermal adsorption-desorption. The results suggested that the crystalline phase of the precursors could be changed with the addition of ionic liquid. By adjusting the content of [Bmim]BF₄, the precursors could be transformed from γ-AlOOH to the mixture of gibbsite and diopside. The final alumina products were obtained after high temperature calcination and the structural transformation of alumina from rhombohedral nanosheets to hexagonal nanoplates were achieved. The well-defined γ-Al₂O₃ hexagonal nanoplates with average diameter of 600 nm and thickness of 200 nm were finally formed after reaction at 160 ℃ for 24 h when the molar ratio of [Bmim]BF₄ to aluminum source was 0.15, and their exposed facets consisted of {111} planes as basal surfaces and {110} planes as lateral surfaces. Compared with the rhombohedral nanosheets prepared without [Bmim]BF₄ template, the obtained hexagonal nanoplatests possessed relatively larger specific surface area(203 m²/g) and more uniform mesoporous structure(4.2 nm). Meanwhile, the template effect of [Bmim]BF₄ on the controllable synthesis of γ-Al₂O₃ hexagonal nanoplates was investigated in detail.

Key words: Ionic liquid, Template, Alumina, Hexagonal nanoplate, Controllable synthesis

CLC Number:

O611.62

TrendMD:

LEI Xuanxuan, TANG Shaokun, LI Lin, SUN Liwei. Controllable Synthesis of γ-Al₂O₃ Hexagonal Nanoplates with Ionic Liquids as the Template^†[J]. Chem. J. Chinese Universities, 2018, 39(11): 2372.

Figures/Tables 12

Fig.1 WAXRD patterns of γ-Al2O3 samples synthesized with different concentrations of [Bmim]BF4a. MA-0-24; b. MA-0.05-24; c. MA-0.10-24;d. MA-0.15-24.

Fig.2 SAXRD pattern(A) and FTIR spectrum(B) of MA-0.15-24

Fig.3 Typical SEM images of alumina synthesized with different concentrations of [Bmim]BF4(A), (B) MA-0-24; (C), (D) MA-0.05-24; (E), (F) MA-0.10-24; (G), (H) MA-0.15-24.

Fig.4 Typical TEM images of alumina synthesized with different concentrations of [Bmim]BF4(A) MA-0-24; (B) MA-0.05-24; (C) MA-0.10-24; (D) MA-0.15-24.

Fig.5 HRTEM images of the as-synthesized alumina(A) MA-0-24; (B) MA-0.15-24. The insets are the corresponding Fourier fast transform(FFT) patterns.

Fig.6 Crystallographic simulations of the as-synthesized alumina(A) Rhombohedral nanosheet; (B) hexagonal nanoplate.

Fig.7 N2 adsorption-desorption isotherms(A) and pore-size distribution plots(B) of the as-synthesized aluminaa. MA-0-24; b. MA-0.15-24.

Table 1 Pore parameters of the products synthesized with or without [Bmim]BF4

Sample	S_BET/(m²·g^-1)	D_pore/nm	V_pore/(cm³·g^-1)
MA-0-24	124	22.83	0.73
MA-0.15-24	203	4.42	0.28

Fig.8 SEM images of γ-Al2O3 synthesized at different reaction time (A) MA-0.15-1; (B) MA-0.15-6; (C) MA-0.15-12; (D) MA-0.15-24.

Fig.9 XRD patterns of the as-prepared precursors at different molar ratios of [Bmim]BF4 to aluminum sourcea. MA-0-24; b. MA-0.05-24; c. MA-0.10-24;d. MA-0.15-24.

Fig.10 FTIR spectra of precursor of MA-0.10-24(a), precursor of MA-0-24(b) and pure [Bmim]BF4(c)

Scheme 1 Growth mechanism of γ-Al2O3 hexagonal nanoplate

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Controllable Synthesis of γ-Al₂O₃ Hexagonal Nanoplates with Ionic Liquids as the Template^†

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