-
摘要: 以Ca(OH)2和m-ZrO2为原料，按物质的量1:1配料，添加不同质量分数的CuO，混料均匀后压样在不同烧结温度保温3 h后制备锆酸钙。将烧结后的样品用显气孔体密测定仪、X射线衍射仪（X-ray diffraction，XRD）、扫描电子显微镜（scanning electron microscope，SEM）分析CuO对锆酸钙材料的烧结性能、物相组成、微观结构的影响。结果表明：样品在1600 ℃温度烧结后，当没有添加CuO时，试样烧结前后线收缩率为11.22%，体积密度为3.37 g·cm-3，显气孔率为15.6%，CaZrO3晶粒尺寸为3.58 μm；当加入质量分数为1.5% CuO时，由于在烧结过程中CuO和CaO反应生成低熔点相CaO-CuO，产生液相促进烧结，试样烧结前后线收缩率为19.68%，制备锆酸钙体积密度为4.07 g·cm-3，显气孔率为7.6%，CaZrO3晶粒尺寸为5.14 μm。Abstract: CaZrO3was prepared by solid reaction for 3 h at different sintering temperatures using Ca(OH)2and m-ZrO2(1:1 by mole) as raw materials with the different contents of CuO by mass as additive. The effects of CuO on sintering properties, phase composition, and microstructures of CaZrO3were studied by apparent porosity density determinator, X-ray diffraction (XRD), scanning electron microscope (SEM), and X'Pert plus software. The results show that, CaZrO3can be synthesized by Ca(OH)2and m-ZrO2at 1500 ℃ to 1600 ℃ sintered for 3 h. For the CaZrO3samples without CuO, the sharking is 11.22%, bulk density is 3.37 g·cm-3, apparent porosity is 15.6%, and grain size is 3.58 μm. For the CaZrO3 samples added 1.5% CuO by mass, the sharking is 19.68%, bulk density reaches to 4.07 g·cm-3, apparent porosity is 7.6%, and grain size is 5.14 μm. The reason could be summarized as the low melting reaction product (CaO-CuO) generated by CuO and CaO at high temperature, which could form the liquid at high temperature and promote the sintering.
-
Key words:
- CaZrO3 /
- CuO /
- apparent porosity /
- bulk density
-
图 1 CuO对锆酸钙线变化率的影响
Figure 1. The sharking of CaZrO3materials with different contents of CuO by mass
图 2 CuO对锆酸钙显气孔率和体积密度的影响：（a）1500 ℃；（b）1550 ℃；（c）1600 ℃
Figure 2. Effects of apparent porosity and bulk density on CaZrO3materials with different contents of CuO by mass: (a) 1500 ℃; (b) 1550 ℃; (c) 1600 ℃
图 3 添加不同质量分数CuO试样X射线衍射图谱
Figure 3. XRD of samples with different contents of CuO by mass
图 4 添加不同质量分数CuO试样的扫描电子显微组织形貌：（a）0；（b）0.5%；（c）1.0%；（d）1.5%；（e）2.0%
Figure 4. SEM images of CaZrO3material with different contents of CuO by mass: (a) 0; (b) 0.5%; (c) 1.0%; (d) 1.5%; (e) 2.0%
图 5 添加质量分数1.5%CuO的锆酸钙样品电子扫描显微组织形貌
Figure 5. SEM images of CaZrO3added by CuO with the mass fraction of 1.5%
表 1 CuO质量分数与样品中锆酸钙晶粒尺寸的关系
Table 1. Grain size of CaZrO3particles with different contents of CuO by mass
CuO质量分数/ % 0 0.5 1.0 1.5 2.0 CaZrO3晶粒尺寸/ μm 3.58 4.37 4.79 5.14 4.86 
下载: 导出CSV
-
[1] Nadler M R, Fitzsimmons E S. Preparation and properties of calcium zirconate. J Am Ceram Soc, 1955, 38(6): 214 doi: 10.1111/j.1151-2916.1955.tb14932.x/abstract [2] Yajima T, Kazeoka H, Yogo T, et al. Proton conduction in sintered oxides based on CaZrO3. Solid State Ionics, 1991, 47(3-4): 271 doi: 10.1016/0167-2738(91)90249-B [3] Rij L V, Winnubst L, Jun L, et al. Analysis of the preparation of in-doped CaZrO3 using a peroxo-oxalate complexation method. J Mater Chem, 2000, 10(11): 2515 doi: 10.1039/b003840g [4] Chen D P, Liu F M. The properties of CaZrO3 and its application in refractories. Bull Miner Petrol Geochem, 1999, 18(4): 343 https://www.cnki.com.cn/Article/CJFDTOTAL-KYDH199904036.htm陈德平, 刘凤梅. CaZrO3的性质及其在耐火材料中的应用. 矿物岩石地球化学通报, 1999, 18(4): 343 https://www.cnki.com.cn/Article/CJFDTOTAL-KYDH199904036.htm [5] Ling J D. Introduction of materials based on calcium zirconate. Bull Chin Ceram Soc, 1986, 5(3): 26凌继栋. 锆酸钙质耐火材料简介. 硅酸盐通报, 1986, 5(3): 26 [6] Han J D, Wen Z Y, Zhang J C, et al. CaZrO3 based high temperature proton conductors. Prog Chem, 2012, 24(9): 1845 https://www.cnki.com.cn/Article/CJFDTOTAL-HXJZ201209023.htm韩金铎, 温兆银, 张敬超, 等. 锆酸钙基高温质子导体材料. 化学进展, 2012, 24(9): 1845 https://www.cnki.com.cn/Article/CJFDTOTAL-HXJZ201209023.htm [7] Liang L P, Gao Y B, Chen S Y. Preparation of CaO–ZrO2 ultrafine powder by coprecipitation-supercritical fluid drying method and investigation on its sintering behaviour (Ⅰ) Preparation and characterization of ultrafine powders. Bull Chin Ceram Soc, 1998, 17(3): 17 https://www.cnki.com.cn/Article/CJFDTOTAL-GSYT803.003.htm梁丽萍, 高荫本, 陈诵英. 共沉淀–超临界流体干燥法合成CaO–ZrO2复合氧化物超微粉体及其烧结性能研究(Ⅰ)粉体的制备及性能表征. 硅酸盐通报, 1998, 17(3): 17 https://www.cnki.com.cn/Article/CJFDTOTAL-GSYT803.003.htm [8] Li W, Zhou G J, Zhang A Y, et al. Preparation and luminescence properties of rare earth-doped calcium zirconate nanocrystal. J Chin Ceram Soc, 2011, 39(11): 1729 https://www.cnki.com.cn/Article/CJFDTOTAL-GXYB201111005.htm李玮, 周广军, 张爱玉, 等. 稀土离子掺杂锆酸钙纳米晶的制备及发光性质. 硅酸盐学报, 2011, 39(11): 1729 https://www.cnki.com.cn/Article/CJFDTOTAL-GXYB201111005.htm [9] You J G, Zhang G D, Jin Y L, et al. Effect of SiO2 on structure and properties of CaZrO3 Material. J Synth Cryst, 2014, 43(5): 1280 doi: 10.3969/j.issn.1000-985X.2014.05.044游杰刚, 张国栋, 金永龙, 等. 二氧化硅对锆酸钙材料结构及性能的影响. 人工晶体学报, 2014, 43(5): 1280 doi: 10.3969/j.issn.1000-985X.2014.05.044 [10] You J G, Zhang G D, Gao P L, et al. Effect of Al2O3 addition on composition and structure of CaZrO3 synthesized from ZrO2 and CaCO3. Trans Mater Heat Treat, 2014, 35(5): 39 https://www.cnki.com.cn/Article/CJFDTOTAL-JSCL201405008.htm游杰刚, 张国栋, 高配亮, 等. 氧化铝对锆酸钙材料组成和结构的影响. 材料热处理学报, 2014, 35(5): 39 https://www.cnki.com.cn/Article/CJFDTOTAL-JSCL201405008.htm [11] Zhang W N, Deng N, Liang W J, et al. Effect of CuO on the sintering properties of dolomite. Powder Metall Technol, 2016, 34(4): 277 doi: 10.3969/j.issn.1001-3784.2016.04.008张汪年, 邓宁, 梁伟杰, 等. CuO对白云石烧结性能的影响. 粉末冶金技术, 2016, 34(4): 277 doi: 10.3969/j.issn.1001-3784.2016.04.008 -
点击查看大图
计量
- 文章访问数: 259
- HTML全文浏览量: 112
- PDF下载量: 9
- 被引次数: 0
