烧结助剂中CaO质量分数及烧结温度对氧化铝基微波陶瓷性能的影响

亢静锐; 董桂霞; 韩伟丹; 李雷; 吕易楠; 张茜

doi:10.19591/j.cnki.cn11-1974/tf.2018.01.002

烧结助剂中CaO质量分数及烧结温度对氧化铝基微波陶瓷性能的影响

doi: 10.19591/j.cnki.cn11-1974/tf.2018.01.002

亢静锐^{1, 2},
董桂霞^{1, 2, ,},
韩伟丹^{1, 2},
李雷^{1, 2},
吕易楠^{1, 2},
张茜^{1, 2}

1.
华北理工大学材料科学与工程学院，唐山 063210
2.
河北省无机非金属材料重点实验室，唐山 063210

基金项目:

国家国际科技合作计划项目 2014DFR50570

详细信息

通讯作者:
董桂霞, E-mail: dgxdgx01@163.com

中图分类号: TQ174
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- 被引次数: 0
出版历程
- 收稿日期: 2017-05-05
- 刊出日期: 2018-02-27

Influence of CaO content by mass in sintering aid and sintering temperature on the properties of Al₂O₃-based microwave ceramic materials

KANG Jing-rui^{1, 2},
DONG Gui-xia^{1, 2
, ,},
HAN Wei-dan^{1, 2},
LI Lei^{1, 2},
LV Yi-nan^{1, 2},
ZHANG Xi^{1, 2}

1.
School of Materials Science and Engineering, North China University of Science and Technology, Tangshan 063210, China
2.
Hebei Provincial Key Laboratory of Inorganic Nonmetallic Materials, Tangshan 063210, China

More Information

Corresponding author: DONG Gui-xia, E-mail: dgxdgx01@163.com

摘要

摘要: 选用CaO–SiO₂–TiO₂作为氧化铝陶瓷的烧结助剂，在空气气氛下经过常压烧结制备Al₂O₃陶瓷。研究了烧结助剂中CaO质量分数以及烧结温度对Al₂O₃基微波陶瓷的相组成、微观结构和介电性能的影响。结果表明：添加含CaO烧结助剂的Al₂O₃陶瓷中，出现了CaAl₁₂O₁₉第二相，相含量随着CaO质量分数的增加而增加；随着烧结助剂中CaO质量分数的增加，Al₂O₃陶瓷试样介电常数增大，品质因数先升高后降低。随着烧结温度的升高，Al₂O₃陶瓷相对密度和品质因数先升高后降低，介电常数和谐振频率温度系数增大。当烧结温度为1450 ℃、烧结助剂中CaO质量分数为0.4%时，烧结体的相对密度达到最大值98.61%，介电常数为9.88，品质因数值为21957 GHz，谐振频率温度系数为-21.353×10^-6/℃。
- 氧化铝陶瓷 /
- 烧结助剂 /
- 烧结温度 /
- 相对密度 /
- 介电性能
Abstract: Alumina ceramics were prepared by normal pressure sintering in air, using CaO–SiO₂–TiO₂as the sintering aid. The effects of CaO content by mass in sintering aid and sintering temperature on phase composition, microstructures, and dielectric properties of Al₂O₃-based microwave ceramic samples were investigated. The results show that, the second phase of CaAl₁₂O₁₉appears in the Al₂O₃ceramics with CaO addition, and the phase content increases with the increase of CaO content in sintering aid. The dielectric constant of Al₂O₃ceramics increases with the increase of CaO content in sintering aid, while the quality factor increases first and then decreases. With the increase of sintering temperature, the relative density and quality factor of Al₂O₃ceramics increase first and then decrease, while the dielectric constant and temperature coefficient of resonance frequency keep increasing. The Al₂O₃ceramic sintered at 1450 ℃ with the CaO mass fraction of 0.4% in sintering aid presents the superior comprehensive properties, the relative density of the sintered body is 98.61%, the dielectric constant is 9.88, the quality factor is 21957 GHz, and the temperature coefficient of resonance frequency is -21.353×10^-6/℃.
- alumina ceramics /
- sintering aid /
- sintering temperature /
- relative density /
- dielectric properties

HTML全文

图 1 添加不同质量分数CaO烧结助剂的Al₂O₃陶瓷（1450℃烧结4h）X射线衍射图谱

Figure 1. XRD patterns of Al₂O₃ceramics sintered at 1450℃ for 4h doped with different mass fraction of CaO in sintering aid

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图 2 添加不同质量分数CaO烧结助剂的Al₂O₃陶瓷在1450℃烧结4h的扫描电子显微形貌：（a）0%；（b）0.4%；（c）0.8%；（d）1.2%；（e）1.6%

Figure 2. SEM morphology of Al₂O₃ceramics doped with different mass fraction of CaO in sintering aid sintered at 1450℃ for 4h: (a) 0%; (b) 0.4%; (c) 0.8%; (d)1.2%; (e) 1.6%

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图 3 不同温度下烧结4h的Al₂O₃陶瓷扫描电子显微形貌：（a）1400℃；（b）1450℃；（c）1500℃；（d）1550℃

Figure 3. SEM morphology of Al₂O₃ceramics at different sintering temperatures for 4h: (a) 1400℃; (b) 1450℃; (c) 1500℃; (d) 1550℃

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图 4 添加不同质量分数CaO烧结助剂，在不同温度下烧结4h得到的Al₂O₃陶瓷相对密度

Figure 4. Relative density of Al₂O₃ceramics with different mass fraction of CaO in sintering aid at different sintering temperature for 4h

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图 5 添加不同质量分数CaO烧结助剂，在不同温度下烧结4h得到的Al₂O₃陶瓷样品的介电常数（a）和介电损耗（b）

Figure 5. Dielectric constant (a) and dielectric loss (b) of Al₂O₃ceramics with different mass fraction of CaO in sintering aid at different sintering temperature for 4h

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图 6 添加不同质量分数CaO烧结助剂，在不同温度下烧结4h得到的Al₂O₃陶瓷样品品质因数

Figure 6. Quality factor of Al₂O₃ceramics with different mass fraction of CaO as sintering aid in different sintering temperature for 4h

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图 7 添加不同质量分数CaO烧结助剂，在1450℃下烧结4h得到的Al₂O₃陶瓷样品谐振频率温度系数

Figure 7. Temperature coefficient of resonant frequency of Al₂O₃ceramics sintered at 1450℃ for 4h with different mass fraction of CaO in sintering aid

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表 1 图 2（e）中区域1和区域2能谱分析

Table 1. EDS analysis of area 1 and area 2 in Fig. 2(e)

位置	元素原子数分数/ %
位置	O	Al	Ti	Ca
1	59.72	40.20	0.08	―
2	54.71	37.32	2.20	5.77

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表 2 添加不同质量分数CaO烧结助剂，在不同温度下烧结4h得到的Al₂O₃陶瓷样品中心频率

Table 2. Center response frequency of Al₂O₃ceramics with different mass fraction of CaO in sintering aid at different sintering temperature for 4h

CaO质量分数/ %	中心频率/ GHz
CaO质量分数/ %	1400℃	1450℃	1500℃	1550℃
0	9.34	9.36	9.30	9.25
0.4	9.35	9.42	9.48	9.46
0.8	9.32	9.38	9.44	9.44
1.2	9.33	9.30	9.28	9.27
1.6	9.40	9.38	9.46	9.36

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