CaO-B2O3玻璃助烧的零膨胀系数β-锂霞石陶瓷的制备及性能研究

doi:10.15541/jim20170229

摘要/Abstract

摘要：

采用固相反应法制备CaO-B₂O₃玻璃（简称“CB”玻璃）助烧的零膨胀系数β-锂霞石陶瓷。通过差示扫描量热(DSC)、X射线衍射(XRD)、扫描电子显微镜(SEM)手段分别对CB玻璃的热学特性和助烧后的β-锂霞石陶瓷样品的物相与显微形貌进行表征。结果表明, CB玻璃具有良好的助烧效果, 可以显著降低β-锂霞石陶瓷的烧结温度(从1300℃降至1150℃), 并大幅提高陶瓷的相对密度(从93.3%提高到97.4%)。加入CB玻璃助烧剂, β-锂霞石陶瓷致密性显著提高, 内部无微裂纹存在。加入4wt%和6wt% CB玻璃的β-锂霞石陶瓷在室温~200℃范围内具有零膨胀系数, 分别为0.02×10^-6/K和0.4×10^-6/K。然而, 加入8wt% CB玻璃的β-锂霞石陶瓷样品中产生了具有高正膨胀系数的新物相LiAlO₂, 使样品的热膨胀系数提高至3.46×10^-6/K。

关键词: β-锂霞石;, CaO-B₂O₃玻璃, 微裂纹, 热膨胀系数

Abstract:

β-eucryptite ceramics with zero coefficient of thermal expansion (CTE) were prepared via solid state reaction method, adding CaO-B₂O₃ glass (CB glass) as sintering aid. The thermal property of CB glass and the crystalline phase, micro-structure of β-eucryptite ceramic samples were investigated by differential scanning calorimetry (DSC), X-ray diffraction (XRD) and scanning electron microscope (SEM), respectively. The results indicate that CB glass is a good sintering aid. It significantly decreased the sintering temperature of β-eucryptite ceramics (from 1300℃ to 1150℃) and increased the relative bulk density (from 93.3% to 97.5%). No micro-cracks were found in β-eucryptite ceramics aided with CB glass. β-eucryptite ceramics added with 4wt%, 6wt% CB glass possessed zero CTE of 0.02×10^-6/K and 0.4×10^-6/K ranging from room temperature to 200℃, respectively. However, a new phase LiAlO₂ with extremely high positive CTE appears in the β-eucryptite ceramics added with 8wt% CB glass which leads to a positive CTE of 3.46×10^-6/K.

Key words: β-eucryptite;, CaO-B₂O₃ glass, micro-crack, coefficient of thermal expansion

中图分类号:

TQ174

姚晓刚, 任海深, 姜少虎, 张奕, 顾忠元, 林慧兴. CaO-B₂O₃玻璃助烧的零膨胀系数β-锂霞石陶瓷的制备及性能研究[J]. 无机材料学报, 2018, 33(4): 385-389.

YAO Xiao-Gang, REN Hai-Shen, JIANG Shao-Hu, ZHANG Yi, GU Zhong-Yuan, LIN Hui-Xing. Preparation and Property of β-eucryptite Ceramics Possessing Zero Coefficient of Thermal Expansion with CaO-B₂O₃ Glass as Sintering Aid[J]. Journal of Inorganic Materials, 2018, 33(4): 385-389.

图/表 6

图1 CB玻璃的DSC曲线

Fig. 1 DSC curve of CB glass

图2 LCx(x=0, 2, 4, 6, 8)陶瓷样品密度与烧结温度的关系曲线

Fig. 2 Relationship between bulk density of LCx (x=0, 2, 4, 6, 8) ceramic samples and sintering temperature

表1 LCx(x=0, 2, 4, 6, 8)陶瓷样品的烧结温度、密度与热膨胀系数

Table 1 Sintering temperature, density and thermal expansion coefficient of LCx (x=0, 2, 4, 6, 8) ceramic samples

Sample	T_s/℃	Density/(g•cm^-3)	CTE/(×10^-6, K^-1)
LC₀	1300	2.233	-4.59
LC₂	1250	2.287	-2.41
LC₄	1200	2.316	0.02
LC₆	1175	2.332	0.48
LC₈	1150	2.336	3.45

图3 LCx(x=0, 6, 8)陶瓷样品的粉末X射线衍射图谱

Fig. 3 Powder X-ray diffraction patterns of LCx(x=0, 6, 8) ceramic samples

图4 LCx(x=0, 2, 4, 6, 8)陶瓷样品的断面SEM照片

Fig. 4 Cross section SEM images of LCx (x=0, 2, 4, 6, 8) ceramic samples

图5 (a) LCx(x=0, 2, 4, 6, 8)陶瓷样品的热膨胀曲线(25~200℃), (b) 放大的LC4和LC6陶瓷样品热膨胀曲线

Fig. 5 (a) Thermal expansion curves of LCx(x=0, 2, 4, 6, 8) ceramic samples with (b) enlarged thermal expansion curves of LC4 and LC6 ceramic samples

参考文献 15

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CaO-B₂O₃玻璃助烧的零膨胀系数β-锂霞石陶瓷的制备及性能研究

Preparation and Property of β-eucryptite Ceramics Possessing Zero Coefficient of Thermal Expansion with CaO-B₂O₃ Glass as Sintering Aid

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