Effects and Oxidation Kinetics of Holding Time on the β-Sialon Bonded MgAl2O4-C Composites

doi:10.15541/jim20160419

Abstract

Abstract:

A β-Sialon bonded MgAl₂O₄-C refractory was prepared in-situ by fused spinel, silicon powder, flake graphite as raw materials, and calcium lignosulfonate with the concentration of 1.25 g/mL as the binder. The samples were sintered under N₂ atmosphere at 1450℃ for 1, 2 3 and 4 h, respectively. The effects of holding time on the conventional physical properties, phase compositions and microstructure of MgAl₂O₄-C refractory were investigated. The phase composition and microstructure of the sintered samples were investigated by X-ray diffraction (XRD) and Scanning Electron Microscope (SEM), respectively. XRD patterns showed that there were no evident differences on the phase compositions and the silicon phase had completely disappeared to form SiC, Si₃N₄ or β-Sialon (Si₃Al₃O₃N₅). The β-Sialon crystals had columned microstructure stagger on each other when holding time was 3 h. With the holding time increasing from 1 h to 4 h, the increased SiO gas lead to an increase of apparent porosity and a decrease of bulk density. In addition, the cold crushing strength and flexural strength of the samples sintered at 1450℃ for 3 h reach the highest. Research on oxidation kinetics of composite material indicates that oxidation process can be divided into three stages: chemical reaction rate controlling stage, diffusion rate controlling stage, and co-effect controlling of chemical reaction and diffusion rate stage.

Key words: β-Sialon bonded MgAl2O4-C refractory, in-situ, holding time, oxidation kinetics

SONG Yun-Fei, WANG Shao-Hua, DENG Cheng-Ji, ZHU Hong-Xi, LIU Jian-Peng, DING Jun, YU Chao. Effects and Oxidation Kinetics of Holding Time on the β-Sialon Bonded MgAl₂O₄-C Composites[J]. Journal of Inorganic Materials, 2017, 32(5): 495-501.

Figures/Tables 9

Table 1 Experimental formula of MgAl2O4-C materials

Materials	Size/mm	wt/%
Fused spinel	1-3	40
	≤1	30
	≤0.088	10
Flake graphite	≤0.088	10
Silicon powder	≤0.074	10
Calcium lignosulfonate	1.25 g/mL	4

Fig. 1 XRD patterns of samples nitride at 1450℃ for 1 h (a), 2 h (b), 3 h (c) and 4 h (d)

Table 2 Relationship between Z and d values from the theoretical and experimental results

Crystal face symbols	d/nm
	XRD results	Theoretical results
		Z=2	Z=3	Z=4
(2 0 0)	0.332011	0.331674	0.33284	0.33401
(1 0 1)	0.270064	0.270081	0.272096	0.27411
(2 1 0)	0.251264	0.250722	0.251604	0.25249

Fig. 2 Morphologies of β-Sialon crystals in sintered specimens at 1450℃ with different holding time

Fig. 3 TEM images of β-Sialon nitridized at 1450℃ for 1 h

Fig. 4 Effects of holding time on the apparent porosity, bulk density, cold crushing strength and flexural strength of the sample

Fig. 5 SEM image of specimen oxidized at 1200℃ for 4 h

Fig. 6 (a) Oxidation kinetics of curves at constant temperatures, (b) oxidizing kinetic curves controlled by chemical reaction rate, (c) oxidizing kinetic curves controlled by interfacial chemical reaction and diffusion rate and (d) oxidizing kinetic curves controlled by diffusion rate of specimens SMAC

Fig. 7 Effect of constant oxidation temperatures on the oxidationrate constant of SMAC specimens

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Effects and Oxidation Kinetics of Holding Time on the β-Sialon Bonded MgAl₂O₄-C Composites

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