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摘要: 以分析纯Ca(OH)2和m-ZrO2为原料, 按物质的量1:1进行配料, 添加不同质量分数Fe2O3粉末作为添加剂, 经充分混合后压制成ø20 mm×20 mm圆柱试样, 再经1600℃保温3 h煅烧制备得到锆酸钙陶瓷试样(CaZrO3)。利用显气孔体密测定仪、X射线衍射仪及扫描电子显微镜分析Fe2O3粉末添加剂对CaZrO3陶瓷材料烧结性能、物相组成及微观结构的影响。结果表明:当没有添加Fe2O3粉末时, 试样烧结前后线变化率为12.72%, 体积密度为3.92g·cm-3, 显气孔率为14.9%, CaZrO3晶粒尺寸为4.22μm; 当加入质量分数0.75%Fe2O3粉末时, 试样烧结前后线变化率为17.20%, 体积密度为4.68 g·cm-3, 显气孔率为6.8%, CaZrO3晶粒尺寸为5.21μm。Abstract: Using analytical Ca(OH)2 and m-ZrO2 as the raw materials in the mole ratio of 1:1, the compacted cylinder samples of calcium zirconate (CaZrO3) ceramics in the dimension of ø20 mm × 20 mm were synthetized by sintering at 1600 ℃ for 3 h, adding the Fe2O3 powders in different mass fractions as the additive agent.The effects of Fe2O3 additive agent on sintering properties, phase composition, and microstructures of CaZrO3 ceramics were studied by apparent porosity density determinator, X-ray diffraction (XRD) diffractometer, and scanning electron microscope (SEM).The results show that, without the addition of Fe2O3, the sharking of CaZrO3 samples is 12.72%, the bulk density and apparent porosity of sintered CaZrO3 samples at 1600 ℃ are 3.92 g·cm-3 and 14.9%, respectively, and the grain size of CaZrO3 is only 4.22 μm.With the addition of Fe2O3 in mass fraction of 0.75%, the sharking of CaZrO3 samples is 17.20%, the bulk density and apparent porosity of sintered CaZrO3 samples at 1600 ℃ are 4.68 g·cm-3 and 6.8%, respectively, and the grain size of CaZrO3 reaches to 5.21 μm.
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Key words:
- calcium zirconate ceramics /
- additive agent /
- bulk density /
- apparent porosity /
- phase composition /
- microstructures
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图 1 烧结前后试样线变化率与添加Fe2O3质量分数的关系
Figure 1. Relationship between the shrinkage of samples before and after sintering and the addition content of Fe2O3 by mass
图 2 烧结试样体积密度、显气孔率与添加Fe2O3质量分数的关系
Figure 2. Relationship of bulk density, apparent porosity, and addition content of Fe2O3 by mass of sintering samples
图 3 添加不同质量分数Fe2O3试样的X射线衍射图谱
Figure 3. XRD pattern of samples added by Fe2O3 in different mass fractions
图 4 添加不同质量分数Fe2O3的CaZrO3试样在1600℃烧结后扫描电子显微形貌: (a) 0%; (b) 0.25%; (c) 0.50%; (d) 0.75%; (e) 1.00%; (f) 1.25%
Figure 4. SEM images of sintered CaZrO3 samples at 1600℃added by Fe2O3 in different mass fractions: (a) 0%; (b) 0.25%; (c) 0.50%; (d) 0.75%; (e) 1.00%; (f) 1.25%
图 5 添加不同质量分数Fe2O3烧结试样的X射线衍射图谱
Figure 5. XRD patterns of sintered samples added by Fe2O3 in different mass fractions
图 6 添加质量分数1.00%Fe2O3的试样烧结后扫描电子显微形貌
Figure 6. SEM images of sintered samples added by Fe2O3 in the mass fractions of 1.00%
表 1 Fe2O3质量分数与CaZrO3晶粒直径的关系
Table 1. Relationship between CaZrO3 particle diameter and the addition content of Fe2O3 by mass
Fe2O3质量分数/ % 0 0.25 0.50 0.75 1.00 1.25 CaZrO3晶粒直径/ μm 4.22 4.45 4.98 5.21 5.04 4.89 
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表 2 图 6晶界处(位置1)和晶粒处(位置2)能谱分析
Table 2. Energy spectrum analysis of crystal boundary (position 1) and crystal particle (position 2) in Fig.6
元素 晶界处成分（位置1） 晶粒处成分（位置2） 质量分数/ % 原子数分数/ % 质量分数/ % 原子数分数/ % O 32.13 66.66 38.25 72.53 Ca 18.29 15.14 16.92 12.78 Zr 48.90 17.79 44.82 14.87 Fe 0.68 0.40 0 0 总计 100 100 100 100
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