晶界非晶结构对Sialon陶瓷多层次相关系的调控: 回顾与展望

doi:10.15541/jim20170452

摘要/Abstract

摘要：

Sialon陶瓷相图和Si₃N₄陶瓷晶界非晶层是陶瓷学科独立发展后两个具有代表性的基础研究高峰。虽然这两类陶瓷只在成分上体现出细小的差异, 并且在实际应用甚至微结构研究时大多将其忽略, 但反映出相图与晶界在结构层次、研究思路和方法上的鸿沟。进入本世纪后, 本颗题组在发展针对微区成分的分析电镜技术的同时, 尝试将Sialon陶瓷的相图和微结构通过掺杂物的分布规律开展协同研究, 获得了晶界非晶成分与相关系的多种联系。这为Sialon陶瓷相变机理研究开辟了新的可能, 也为陶瓷体系的跨尺度结构-性能关系预测、设计与全周期调控提供了不同的研究思路。

关键词: Sialon陶瓷, 相图, 晶界结构, 分析电镜, 相变, 综述

Abstract:

Phase diagram in Sialon ceramics and intergranular amorphous films in Si₃N₄ ceramics, are two successful aspects for fundamental studies in ceramic as an independent discipline. Although differing only in secondary compositions, the small gap in stoichiometry between the two systems divides structure, scale and scope in ceramic research. Started from this century, a series of analytical TEM methodology to probe into local composition within individual grains and even inside grain-boundaries have been developed. This provides the possibility to unify the phase diagram and intergranular structure in Sialon ceramics, especially for them to connect and correlate into a multi-levelled structure framework, which can develop not only an alternative approach to study phase transformation, but also a hierarchical structure-property relationship that serves the full-life circle of ceramic materials.

Key words: Sialon ceramics, phase diagram, intergranular structures, analytical TEM, phase transformation, review

中图分类号:

TQ174

顾辉. 晶界非晶结构对Sialon陶瓷多层次相关系的调控: 回顾与展望[J]. 无机材料学报, 2018, 33(2): 147-152.

GU Hui. Correlation of Intergranular Amorphous Structures on Multi-levelled Phase Relationship in Sialon Ceramics: Retrospect and Prospect[J]. Journal of Inorganic Materials, 2018, 33(2): 147-152.

图/表 10

图1 稀土固溶范围与半径关系[23]

Fig. 1 Early study of RE solid-solution in α-Sialon[23]

图2 三个不同Nd-α-Sialon样品各晶粒固溶度对比[21]

Fig. 2 Comparison of solid-solution in different grains from 3 Nd-α-Sialon samples[21]

图3 Nd-α-Sialon微结构中的晶界非晶相(TP, ~10 nm三叉晶界; QP, ~100 nm四岔晶界)[21]

Fig. 3 Intergranular amorphous pockets in Nd-α-Sialon(TP~ 10 nm, QP~100 nm)[21]

图4 Nd-α-Sialon陶瓷中QP非晶相成分[21]

Fig. 4 Compositions measured from amorphous QP regions in Nd-α-Sialon[21]

图5 Ca-Al-Si-O-N五元相图中的Sialon相截面[27]

Fig. 5 Sialon-section in Ca-Al-Si-O-N phase prism[27]

图6 Ca-α-Sialon系列样品晶粒中固溶度测量[22]

Fig. 6 Solid-solutions measured from Ca-α-Sialon grains[22]

表1 Ca-α-Sialon陶瓷的名义与实测固溶值[22]

Table 1 Nominal (x) and measured values by EPMA and AEM in Ca-α-Sialon ceramics[22]

	x	EPMA	AEM	Extra phase
CA03	0.3	-	0.25 (6)	β
CA06	0.6	0.4	0.36 (6)	-
CA10	1.0	0.7	0.64 (7)	21R
CA14	1.4	0.9	0.48 (5)	21R

图7 Ca-α-Sialon晶界偏析元素探测[22]

Fig. 7 Segregation detection at GB in Ca-α-Sialon[22]

图8 Ca-α-Sialon陶瓷晶粒中实测固溶量变化规律(实线)与设计固溶量(虚线)对比图[20]

Fig. 8 Solid-solutions measured from individual grains (solid lines) and designed (dotted lines) in Ca-α-Sialon ceramics[20]

图9 Nd-α-Sialon陶瓷晶界非晶层中的偏析成分与相邻的晶界非晶相有关, 并形成梯度[20]

Fig. 9 Gradient of dopant segregation to grain-boundary subject to neighboring inter-granular glassy pockets in Nd-α-Sialon ceramics[20]

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