Effects of Gel Aging on Synthesis of ZrB2 Powders

doi:10.3724/SP.J.1077.2014.13564

Abstract

Abstract:

ZrB₂ particles were synthesized by a Sol-Gel method using zirconium n-propoxide, boric acid, acetic acid and D-fructose. D-Fructose acts as both a modifier and a carbon source for carbothermal reduction reaction. For comparison, both nascent state gel and aged gel were used to clarify the aging-time-dependent mechanism for ZrB₂ synthesis. As a result, a single phase ZrB₂ powder with a uniform size and shape distribution can be obtained from the aged gel with a boron and carbon to zirconium molar ratio of 3.5-4 and 7, respectively, after reduced at 1550 ℃ for 2 h. Besides, the synthesized ZrB₂ particles exhibit prism-like morphology with average particle size of ca. 4-7 μm in length, 1 μm in diameter of excircle of the cross-section and 4-7 in aspect ratio, when initial raw materials ratio n(B)/n(Zr) is 3.5-4 and n(C)/n(Zr) is 7. The median diameter D₅₀ is 6.46 μm and specific surface area is about 2.53 m²/g. Furthermore, a complete carbothermal reduction of ZrO₂ can be achieved using the aged gel.

Key words: aging, Sol-Gel, synthesis, ZrB2

CLC Number:

TQ174

YANG Bi-Yun, LI Jun-Ping, WANG Ting-Yu, LI Rui-Xing, FENG Zhi-Hai, CAI Hong-Nian. Effects of Gel Aging on Synthesis of ZrB₂ Powders[J]. Journal of Inorganic Materials, 2014, 29(7): 717-721.

Figures/Tables 8

Fig. 1 Flow chart for the synthesis of ZrB2 powder

Fig. 2 XRD patterns of ZrB2 powders calcined at 1550 ℃ for 2 h using nascent state gels Molar ratios of (a) B/Zr = 3.5, C/Zr = 5; (b) B/Zr = 3.5, C/Zr = 7; (c) B/Zr = 4, C/Zr = 7

Fig. 3 XRD patterns of ZrB2 powders calcined at 1550 ℃ for 2 h using nascent state gels with n(C)/n(Zr)= 8 and different B/Zr molar ratios of (a) 3.5 and (b) 4

Fig. 4 XRD patterns of ZrB2 powders calcined at 1550 ℃ for 2 h using aged gels with n(C)/n(Zr) = 7 and different B/Zr molar ratios of 3.5 (a) and 4 (b)

Fig. 5 XRD patterns of ZrB2 powders calcined at (a) 1300 ℃ and (b) 1550 ℃ for 2 h using aged gels with molar ratios of B/Zr = 3.5 and C/Zr = 7

Fig. 6 SEM image of ZrB2 powders calcined at 1550 ℃ for 2 h using the aged gel with molar ratios of B/Zr = 3.5 and C/Zr = 7

Fig. 7 Particle size distribution of ZrB2 powders calcined at 1550 ℃ for 2 h using the aged gel with molar ratios of B/Zr = 3.5 and C/Zr = 7

Table1 Specific surface areas (BET) of ZrB2 powders calcined at 1550 ℃for 2 h using nascent state gels and aged gels with molar ratios of B/Zr = 3.5 and C/Zr = 7

Sample	Gel	BET/(m²·g^-1)
1	Nascent state	15.29
2	Aged	2.53

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Effects of Gel Aging on Synthesis of ZrB₂ Powders

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