Mass Production of α-silicon Nitride Single-crystalline Nanowires

doi:10.15541/jim20180381

Abstract

Abstract:

α-silicon nitride single-crystalline nanowires were prepared by direct nitridation of granulation Si powders in N₂-H₂mixture gas. The nitridation product has the core-shell structure (Si₃N₄nanowires @porous Si₃N₄ powders), where Si₃N₄nanowires can be effectively separated by crushing and grinding. The results show that the as-prepared α-Si₃N₄nanowires are straight and uniform with diameters of 80-150 nm, length to diameter ratios of 20-50, purity higher than 95wt%, and yield of 3.1%. Further study indicates that growth of Si₃N₄nanowires is controlled by the Vapor-Liquid-Solid (VLS) mechanism, where the trace Fe elements serves as catalyst in the reduction atmosphere. In this study, The process of the raw silicom powder granulation after nitriding shows three advantages: 1) remarkably increasing growth space of nanowires; 2) leading to concentrated distribution of nanowire, tacilitating subsequent separation; 3) remarkably increasing the nitridation rate.

Key words: Si₃N₄, nanowires, direct nitridation, granulation, VLS mechanism

CLC Number:

TB32

Chao LEI, Fei WEI. Mass Production of α-silicon Nitride Single-crystalline Nanowires[J]. Journal of Inorganic Materials, 2019, 34(6): 667-672.

Figures/Tables 9

Fig. 1 SEM images and photograph of different samples (a) SEM image of Si raw materials; (b) SEM images of Granulation Si powders; (c) SEM image of granulation Si powders after 3 h nitridation; (d) Photograph of Si3N4/ alcohol mixture after stratification

Fig. 2 XRD patterns of Si raw materials, Si3N4 powders, Si3N4 nanowires

Table 1 Impurity elements analysis results

Element/wt%	Fe	Ca	Al	O	C
Si raw materials	0.008	0.013	0.012	0.14	-
Si₃N₄nanowires	0.011	0.007	0.031	1.56	-
Si₃N₄particles	0.006	0.014	0.049	1.07	-

Fig. 3 Morphologies of Si3N4 nanowires

Table 2 Elemental analysis results of Si3N4 nanowires

Spectrum	Element/at%
Spectrum	Si	N	O	Fe
1	41.42	55.43	3.16	0
2	49.17	46.22	4.17	0.45

Fig. 4 Morphologies under different magnifications for Si3N4 particles

Fig. 5 Morphologies of nanowires on the granulation Si powder surface (a-b) 15 min nitridation in the 90vol% N2-10vol% H2 mixture gas; (c) 3 h nitridation in N2

Fig. 6 SEM images of different Si powders after 3 h nitridation in the 90vol% N2+10vol% H2 mixture gas (a) Raw Si powders; (b) Inside of the granulation Si powders

Fig. 7 Nitridation rate of granulation Si powders at different atmospheres

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