Rapid Synthesis of Mesoporous Nickel Phosphates under Microwave Assisted Hydrothermal Condition

doi:10.3724/SP.J.1077.2012.00501

Abstract

Abstract:

Mesostructured nickel phosphate (MW-NiPO-2) was rapidly synthesized in the presence of cationic surfactant by a microwave assisted hydrothermal process. The synthesis parameters, microwave irradiation temperature and time, OH^-/P and Ni/P molar ratios of the precursor, were systematically investigated and optimized. The characterizations of the materials obtained by the two different procedures, Sol-Gel method and microwave assisted hydrothermal process, were carried out by ICP, FT-IR, TEM and N₂ physisorption. The results show that MW-NiPO-2 can be obtained at relatively low temperature (60℃). When the microwave radiation temperature was 100℃, the mesostructured phase formed in an extremely short period about 0.25 h. Ordered MW-NiPO-2 can be obtained under microwave irradiation for 1 h at 100℃, when OH^-/P and the Ni/P molar ratios of the precursor are 2.0 and 0.7, respectively. In contrast, it took at least 24 h for completion via Sol-Gel method. MW-NiPO-2 and SG-NiPO-2 possess similar structure and composition while MW-NiPO-2 exhibites a worm-like appearance other than piled nanotubes. In comparison with the sample synthesized via Sol-Gel method, MW-NiPO-2 possesses a relatively high BET surface area (334.4 m²/g) and pore volume (0.318 cm³/g).

Key words: mesoporous nickel phosphate, NiPO, microwave assisted hydrothermal synthesis, Sol-Gel method

CLC Number:

TQ426

LI Xu-Ying, TAN Juan, YANG Jian-Hua, LIU Jing, YANG Fei. Rapid Synthesis of Mesoporous Nickel Phosphates under Microwave Assisted Hydrothermal Condition[J]. Journal of Inorganic Materials, 2012, 27(5): 501-506.

Figures/Tables 9

Fig. 1 XRD patterns of as-synthesized MW-NiPO-2 (a) and SG-NiPO-2 (b) samples

Fig. 2 Effect of radiation temperature on the evolution of Is/I0 of MW-NiPO-2 (Inset is XRD pattern of sample synthesized at 120℃)

Fig. 3 Effect of radiation time on the evolution of Is/I0 of MW-NiPO-2

Fig. 4 XRD patterns of as-synthesized MW-NiPO-2 samples with different OH-/P (a) 1.9; (b) 2.0; (c) 2.1; (d) 2.3

Fig. 5 XRD patterns of MW-NiPO-2 samples synthesized with different Ni/P molar ratios (a) 0.3, (b) 0.5, (c) 0.7, (d) 0.9

Table 1 ICP data of MW-NiPO-2 samples synthesized with different Ni/P molar ratios in initial gel

Ni/P of initial gel	Ni content /wt%	P content /wt%	Ni/P of MW-NiPO-2
0.3	35.10	11.39	1.63
0.5	34.98	11.87	1.55
0.7	37.69	11.97	1.66

Fig. 6 FT-IR spectra of as-synthesized (a) MW-NiPO-2; (b) SG-NiPO-2 MW-Nipo-2 preparation condition OH-/P=2.0, Ni/P=0.7, 100℃/1 h

Fig. 7 TEM images of as-synthesized mesoporous nickel phosphate samples

Fig. 8 Adsorption-desorption isotherm of extracted samples (a) MW-NiPO-2; (b) SG-NiPO-2

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