J. Mater. Sci. Technol. ›› 2019, Vol. 35 ›› Issue (12): 2851-2858.DOI: 10.1016/j.jmst.2019.07.004
• Orginal Article • Previous Articles Next Articles
Ling-yan Lia1, Hui Gua*(), Vesna Šrotb, Peter van Akenb, Joachim Billc*()
Received:
2019-09-26
Online:
2019-12-05
Published:
2019-12-18
Contact:
Gu Hui,Bill Joachim
Ling-yan Li, Hui Gu, Vesna Šrot, Peter van Aken, Joachim Bill. Initial nucleation of amorphous Si-B-C-N ceramics derived from polymer-precursors[J]. J. Mater. Sci. Technol., 2019, 35(12): 2851-2858.
Fig. 1. SAED patterns of Si-B-C-N PDCs: (a) pyrolyzed at 1000?°C (T10), followed by annealing at (b) 1200?°C (TA12), (c) 1400?°C (TA14), (d) 1500?°C (TA15). Crystallization into β-SiC and graphitic structures (G) is marked onto enlarged pattern in (c). (a) and (c) are adapted from Ref. [10].
SiC (nm) | cluster (nm) | |
---|---|---|
T10 | - | ≤ 2 |
TA12 | 3.2?±?0.9 | 3.7?±?1.0 |
TA14 | 4.5?±?1.5 | 4.7?±?1.1 |
TA15 | 4.9?±?1.2 | 4.7?±?1.0 |
Table 1 Sizes of nano-SiC grains and nano-clusters in Si-B-C-N matrix, measured from HRTEM and HAADF images respectively. See examples in Fig. 2.
SiC (nm) | cluster (nm) | |
---|---|---|
T10 | - | ≤ 2 |
TA12 | 3.2?±?0.9 | 3.7?±?1.0 |
TA14 | 4.5?±?1.5 | 4.7?±?1.1 |
TA15 | 4.9?±?1.2 | 4.7?±?1.0 |
Fig. 3. ELNES patterns to compare bonding of Si-B-C-N matrix before and after annealing, together with reference β-SiC, α-Si3N4, h-BN and graphite phases: (a) silicon L2,3, (b) boron K, (c) carbon K, (d) nitrogen K edges.
Si | B | C | N | O | |
---|---|---|---|---|---|
T10* | 23.0 | 7.9 | 42.8?±?0.3 | 20.0?±?0.3 | 6.4?±?1.0 |
TA12 | 22.1?±?0.5 | 8.4?±?0.7 | 44.8?±?1.0 | 17.0?±?0.7 | 7.6?±?1.5 |
TA15 | 19.4?+?0.7 | 9.8?±?1.0 | 44.4?±?0.7 | 18.9?±?1.4 | 7.6?±?2.0 |
Table 2 Compositions of Si-B-C-N matrix in annealed PDCs by EELS analysis over scanning areas of 5-10?nm. Chemical analysis for as-pyrolyzed T10 are listed for comparison (marked by *): Si and B were determined by optical emission spectrometry with inductively coupled plasma excitation (OES-ICP, Perkin Elmer ICP 5500); C, N, O were analyzed by carrier gas heat extraction (CGHE, LECO C S-analyzer 244 and N O-determinater TC436). See text for more details.
Si | B | C | N | O | |
---|---|---|---|---|---|
T10* | 23.0 | 7.9 | 42.8?±?0.3 | 20.0?±?0.3 | 6.4?±?1.0 |
TA12 | 22.1?±?0.5 | 8.4?±?0.7 | 44.8?±?1.0 | 17.0?±?0.7 | 7.6?±?1.5 |
TA15 | 19.4?+?0.7 | 9.8?±?1.0 | 44.4?±?0.7 | 18.9?±?1.4 | 7.6?±?2.0 |
Fig. 4. EELS line-profiling from: (a) TA12, (b) TA14, revealing bright clusters corresponding to SiC, dark to carbon or graphite, and less bright for Si3N4 segregation before the start of nucleation. Elemental distributions are shown in (a) and Si-L2,3 ELNES are given in (b), which sums up starting and ending sections, sp01-06 and sp17-30, respectively corresponding to Si3N4 and SiC phases. HAADF images are also shown in both cases.
Fig. 5. Calculated equilibrium phase diagram in ternary Si-C-N system at constant 10 at.% boron content, 1400?°C and ptotal =1?bar [16]. The star describes the nominal composition of PDC, and cluster compositions are measured from: (a) T10, (b) TA14, (c) TA15 by probing bright/dark clusters in spot or line-scan modes. Average compositions from PDC matrices were also measured by area analysis.
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