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摘要: 以Ca（OH）2和m-ZrO2为原料，按物质的量1：1进行配料，添加不同质量分数的CaCO3微粉，混料均匀后压样，经1600℃保温3 h后制备得到锆酸钙（CaZrO3）。利用显气孔体密测定仪、X射线衍射仪、扫描电子显微镜和X'Pert plus图象处理软件分析CaCO3微粉对锆酸钙材料烧结性能、物相组成及微观结构的影响。结果表明：当没有添加CaCO3微粉时，试样烧结前后线收缩率为8.23%，体积密度为3.40 g·cm-3，显气孔率为14.5%，CaZrO3晶粒尺寸为4.08μm；当加入质量分数为8% CaCO3微粉时，试样烧结前后线收缩率为14.89%，制备锆酸钙体积密度为4.02 g·cm-3，显气孔率为8.6%，CaZrO3晶粒尺寸为5.45μm；由此可见，添加少量CaCO3微粉有利于锆酸钙烧结致密性和晶粒长大。Abstract: Using analytical Ca(OH)2 and m-ZrO2 as the raw materials in the mole ratio of 1:1, the mixtures were added by CaCO3 powders in the different contents by mass, the calcium zirconate (CaZrO3) was synthesized by sintering the compacted samples at 1600 ℃ for 3 h. The effects of CaCO3 powders on sintering properties, phase composition, and microstructures of CaZrO3 were studied by apparent porosity density determinator, X-ray diffraction (XRD), scanning electron microscope (SEM), and X'Pert plus software. The results show that, without the addition of CaCO3, the sharking of CaZrO3 samples is 8.23%, the bulk density and apparent porosity of CaZrO3 sintered at 1600℃ are 3.40 g·cm-3 and 14.5%, respectively, and the grain size of CaZrO3 is only 4.08 μm. With the addition of CaCO3 in mass fraction of 8%, the sharking of CaZrO3 samples is 14.89%, the bulk density and apparent porosity of CaZrO3 sintered at 1600℃ are 4.02 g·cm-3 and 8.6%, respectively, and the grain size of CaZrO3 reaches to 5.45 μm. Thus, it can be seen that the CaCO3 addition in appropriate content can promote the sintering compactness and grain growth of CaZrO3.
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Key words:
- calcium zirconate /
- CaCO3 powders /
- sintering properties /
- phase composition /
- microstructures
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图 2 线变化率与添加CaCO3微粉质量分数的关系
Figure 2. Relationship between shrinkage and the CaCO3 addition content by mass
图 3 烧结试样体积密度、显气孔率与添加CaCO3质量分数的关系
Figure 3. Relationship of bulk density, apparent porosity, and CaCO3 addition content by mass of sintering samples
图 4 添加质量分数10%CaCO3微粉制备样品的X射线衍射图谱
Figure 4. XRD patterns of samples add by CaCO3 powders in the mass faction of 10%
图 5 添加不同质量分数CaCO3微粉的锆酸钙试样在1600 ℃烧结后扫描电子显微组织形貌：（a）0%；（b）2%；（c）4%；（d）6%；（e）8%；（f）10%
Figure 5. SEM micrographs of sintered CaZrO3 samples at 1600 ℃ added by CaCO3 powders in different mass fractions: (a) 0%; (b) 2%; (c) 4%; (d) 6%; (e) 8%; (f) 10%
图 6 添加质量分数8%CaCO3试样在不同温度烧结后X射线衍射图谱
Figure 6. XRD patterns of samples sintered at different temperatures add by CaCO3 powders in the mass faction of 8%
表 1 样品中CaCO3质量分数与锆酸钙晶粒直径的关系
Table 1. Relationship between CaZrO3 particle diameter and CaCO3 addition content by mass
CaCO3质量分数/% 0 2 4 6 8 10 CaZrO3晶粒直径/μm 4.08 4.43 4.88 5.08 5.45 5.21 
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