Synthesis of ZrB2 Nanoparticles by Using Xylitol

doi:10.15541/jim20150481

Abstract

Abstract:

ZrB₂ nanoparticles were synthesized synergistically by Sol-Gel method and carbothermal reduction reaction using zirconium n-propoxide, acetic acid, boric acid and xylitol as starting materials. In the reaction system, xylitol acted as a carbon source for the carbothermal reduction reaction and chelated boron, leading to the formation of coordination compound through its polyhydroxy reaction with boric acid. According to the Fourier Transform infrared spectra and thermal analysis of gel precursor, the effects of sol and gel reaction processes on the carbothermal reduction reaction temperature and gelation time were discussed. The results show that the polyhydroxy compound of xylitol is beneficial to initiate reactions and gelation, which makes the threshold throughout the whole chemical processes easy to overcome. The gel does not need aging treatment and the reaction temperature is lowered. Besides, a single phase of equiaxed ZrB₂ nanoparticles could be obtained from nascent state gel calcined at 1450℃ with n(xylitol)/n(zirconium n-propoxide) of 1.4. The average diameter and oxygen content of ZrB₂ nanoparticles are ca. 50 nm and 1.36wt%, respectively.

Key words: nanoparticles, xylitol, ZrB2, Sol-Gel, synthesis

CLC Number:

TQ174

ZHAO Yue, LI Jun-Ping, WANG Ting-Yu, LI Rui-Xing, FENG Zhi-Hai, CAI Hong-Nian. Synthesis of ZrB₂ Nanoparticles by Using Xylitol[J]. Journal of Inorganic Materials, 2016, 31(6): 597-601.

Figures/Tables 7

Fig. 1 General flow chart for synthesis of ZrB2 powder

Fig. 2 FTIR spectra of (a) boric acid and (b) ZrB2 precursor powder prepared with n(Xylitol)/n(Zr(OPr)4)=1.4

Fig. 3 TG-DSC curves of (a) xylitol and (b) ZrB2 precursor powder prepared with n(Xylitol)/n(Zr(OPr)4)=1.4 under argon flow at a heating rate of 10℃/min

Fig. 4 XRD patterns of the products calcined from precursors at (a) 1200℃, (b) 1300℃, (c) 1400℃ and (d) 1450℃ for 2 h with n(Xylitol)/n(Zr(OPr)4)=1.4

Fig. 5 XRD patterns of the products calcined from precursors at 1450℃ for 2 h with n(X)/n(Zr) of (a) 1, (b) 1.2 and (c) 1.4

Fig. 6 XRD patterns of the products calcined from precursors at 1450℃ for 2 h using (a) nascent state gel and (b) 6 d-aged gel with n(X)/n(Zr) of 1.4

Fig. 7 SEM images of single-phase ZrB2 powder calcined from precursors at 1450℃ for 2 h with n(X)/n(Zr)=1.4

References 16

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Synthesis of ZrB₂ Nanoparticles by Using Xylitol

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