正、反向共沉淀法对Pr2Zr2O7纳米粒子表观活化能的影响

引用本文: 韩锋, 马伟民, 马雷, 孙杨, 史树君, 李晓龙, 管仁国. 正、反向共沉淀法对Pr₂Zr₂O₇纳米粒子表观活化能的影响[J]. 无机化学学报, 2014, 30(4): 811-820. doi: 10.11862/CJIC.2014.089 shu

Citation: HAN Feng, MA Wei-Min, MA Lei, SUN Yang, SHI Shu-Jun, LI Xiao-Long, GUAN Ren-Guo. Effect of the NSC and RSC Co-precipitation Methods on Apparent Activation Energy of Pr₂Zr₂O₇ Nanopowders[J]. Chinese Journal of Inorganic Chemistry, 2014, 30(4): 811-820. doi: 10.11862/CJIC.2014.089 shu

正、反向共沉淀法对Pr₂Zr₂O₇纳米粒子表观活化能的影响

韩锋 ^1, ,
马伟民 ^{1,
,} ,
马雷 ^1,2, ,
孙杨 ^1, ,
史树君 ^1, ,
李晓龙 ^1, ,
管仁国 ^2,

通讯作者: 马伟民 maweimin56@163.com

基金项目:
沈阳市先进陶瓷制备技术及应用重点实验室建设项目(No：F12-259-1-00)资助项目。 (No：F12-259-1-00)

摘要: 以氨水作为沉淀剂,采用正、反向共沉淀法制备Pr₂Zr₂O₇纳米粒子。利用XRD、SEM、TEM、TG-DTA等测试手段表征了样品物相及形貌；研究其制备过程中合成动力学和晶粒生长动力学,采用Doyle-Ozawa法和Kissinger法分别计算正、反向沉淀粒子在主要反应阶段的表观活化能。结果表明：反向沉淀的滴定速率为2mL·min^-1、母盐溶液初始浓度0.05mol·L^-1、反应体系温度273K、pH值11、煅烧温度为1173K,保温2h的条件下获得的样品形貌近球形、无团聚现象、一次粒径约60nm。Pr₂Zr₂O₇前驱体的分解过程分为3个阶段,正、反向粒子各阶段平均表观活化能分别为：71.2、97.8、183.2kJ·mol^-1和45.37、84.34、152.16kJ·mol^-1；晶粒生长活化能分别为19.02和11.95kJ·mol^-1,后者比前者的晶粒生长活化能降低了7.07kJ·mol^-1；反向共沉淀制备工艺优于正向共沉淀法。

关键词:

Pr₂Zr₂O₇纳米粒子;正、反向共沉淀法;微观形貌;合成动力学;表观活化能

English

Effect of the NSC and RSC Co-precipitation Methods on Apparent Activation Energy of Pr₂Zr₂O₇ Nanopowders

1.
1 Key Laboratory for Advanced Ceramics and Application of Shenyang, School of Materials Science and Engineering, Shenyang University of Chemical Technology, Shenyang 110142, China;

Corresponding author: 马伟民 maweimin56@163.com

Received Date: 30 August 2013
Fund Project:
沈阳市先进陶瓷制备技术及应用重点实验室建设项目(No：F12-259-1-00)资助项目。

Abstract: The Pr₂Zr₂O₇ nanoparticles were prepared by using NSC and RSC co-precipitation method with ammonia as precipitant agent. XRD, SEM, TEM and TG-DTA were applied to analysis the crystallization and morphology of the samples. Synthesis kinetics of the preparation process and dynamics of grain growth were studied, and the apparent activation energy was calculated respectively by using Doyle-Ozawa method and the Kissinger method. The results show that the samples topography near spherical, there are no agglomeration and the mean particle size is about 60nm. They were obtained under the conditions of titration rate, 2 mL·min^-1, initial concentration of resolution, 0.05 mol·L^-1, system temperature 273K and calcination at 1173 K for 2 h by RSC. The average apparent activation energy of the particles, obtained by NSC, were 71.2, 97.8 and 183.2 kJ·mol^-1 in each stage and the RSCs were 45.37, 84.34 and 152.16 kJ·mol^-1; the grain growth activation energy of them were 19.02 and 11.95 kJ·mol^-1 respectively, the latter decreases 7.07 kJ·mol^-1 than the former. Reverse co-precipitation preparation technology is better than that of positive co-precipitation method.

Key words:

Pr₂Zr₂O₇ nanoparticle;NSC and RSC co-precipitation method;micro-morphology;synthesis dynamics;apparent activation

1. [1] XIANG Jian-Ying(项建英), CHEN Shu-Hai(陈树海), HUANG Ji-Hua(黄继华), et al. Acta Metall Sin.(金属学报), 2012, 48(8): 965-970[1] XIANG Jian-Ying(项建英), CHEN Shu-Hai(陈树海), HUANG Ji-Hua(黄继华), et al. Acta Metall Sin.(金属学报), 2012, 48(8): 965-970
2. [2] GONG Wen-Biao(宫文彪), LI Yu-Peng(李于朋), LIU Wei (刘威) et al. J. Inorg. Mater. (无机材料学报), 2010, 25(8): 860-864[2] GONG Wen-Biao(宫文彪), LI Yu-Peng(李于朋), LIU Wei (刘威) et al. J. Inorg. Mater. (无机材料学报), 2010, 25(8): 860-864
3. [3] ZHANG Hong-Song(张红松), HU Ren-Xi(胡仁喜), XU Qiang(徐强), et al. Rare Met. Mater. Eng. (稀有金属材料与工程), 2009, 38(2):735-738[3] ZHANG Hong-Song(张红松), HU Ren-Xi(胡仁喜), XU Qiang(徐强), et al. Rare Met. Mater. Eng. (稀有金属材料与工程), 2009, 38(2):735-738
4. [4] ZHU Zheng-Quan(朱正权), HUANG Yong-Zhang(黄永章), LI Xing-Yan(李兴彦). Metall. Funct. Mater. (金属工程材料), 2011, 18(2):79-82[4] ZHU Zheng-Quan(朱正权), HUANG Yong-Zhang(黄永章), LI Xing-Yan(李兴彦). Metall. Funct. Mater. (金属工程材料), 2011, 18(2):79-82
5. [5] Doménech A, Montoya N, Alarcón J. J. Solid State Electrochem. 2012, 16:963-975[5] Doménech A, Montoya N, Alarcón J. J. Solid State Electrochem. 2012, 16:963-975
6. [6] GAO Shuai(郜帅). Thesis for the Doctorate of Harbin Institute of Technology(哈尔滨工业大学硕士论文), 2010.[6] GAO Shuai(郜帅). Thesis for the Doctorate of Harbin Institute of Technology(哈尔滨工业大学硕士论文), 2010.
7. [7] Kharton V V, Naumovich E N, Vecher A A. J. Solid State Electrochem., 1999, 3:61-81[7] Kharton V V, Naumovich E N, Vecher A A. J. Solid State Electrochem., 1999, 3:61-81
8. [8] LIU Zhan-Guo(刘占国). Thesis for the Doctorate of Harbin Institute of Technology(哈尔滨工业大学博士论文), 2009.[8] LIU Zhan-Guo(刘占国). Thesis for the Doctorate of Harbin Institute of Technology(哈尔滨工业大学博士论文), 2009.
9. [9] LU Xi-Rui(卢喜瑞), DONG Fa-Qin(董发勤), HU Song (胡淞), et al. Acta Phys. Sin. (物理学报), 2012, 61(15)1-8[9] LU Xi-Rui(卢喜瑞), DONG Fa-Qin(董发勤), HU Song (胡淞), et al. Acta Phys. Sin. (物理学报), 2012, 61(15)1-8
10. [10] LI Quan(李权), MA Wei-Min(马伟民), MA Lei(马雷), et al. J. Synth. Cryst. (人工晶体学报), 2013, 42(1): 2-77[10] LI Quan(李权), MA Wei-Min(马伟民), MA Lei(马雷), et al. J. Synth. Cryst. (人工晶体学报), 2013, 42(1): 2-77
11. [11] Dhas N A, Patil K C. J. Mater. Chem., 1993, 3(12):1289-1294[11] Dhas N A, Patil K C. J. Mater. Chem., 1993, 3(12):1289-1294
12. [12] Matsuhira K, Sekine C, Paulsen C, et al. J. Physics: Conf. Series 145(2009) 012031[12] Matsuhira K, Sekine C, Paulsen C, et al. J. Physics: Conf. Series 145(2009) 012031
13. [13] LU Jing(卢靖), HUANG Jian-Feng(黄剑锋), CAO Li-Yun (曹丽云), et al. Chinese J. Inorg. Chem. (无机化学学报), 2013, 29(1):69-74[13] LU Jing(卢靖), HUANG Jian-Feng(黄剑锋), CAO Li-Yun (曹丽云), et al. Chinese J. Inorg. Chem. (无机化学学报), 2013, 29(1):69-74
14. [14] Otero T F, Martinez J G. J. Solid State Electrochem. 2011, 15:1169-1178[14] Otero T F, Martinez J G. J. Solid State Electrochem. 2011, 15:1169-1178
15. [15] SI Wei (司伟), GAO Hong(高宏), WANG Jing(王晶), et al. Chinese J. Inorg. Chem. (无机化学学报), 2010, 26(8), :1443-1449[15] SI Wei (司伟), GAO Hong(高宏), WANG Jing(王晶), et al. Chinese J. Inorg. Chem. (无机化学学报), 2010, 26(8), :1443-1449
16. [16] XIAO Jin(肖劲), DENG Song-Yun(邓松云), WU Sheng-Hui (吴胜辉), et al. Chinese J. Inorg. Chem. (无机化学学报), 2010, 26(3):464-468[16] XIAO Jin(肖劲), DENG Song-Yun(邓松云), WU Sheng-Hui (吴胜辉), et al. Chinese J. Inorg. Chem. (无机化学学报), 2010, 26(3):464-468
17. [17] GUO Yi-Fen(郭易芬), MA Wei-Min(马伟民), WEN Lei (闻雷), et al. Chinese J. Inorg. Chem. (无机化学学报), 2009, 25(5):880-885[17] GUO Yi-Fen(郭易芬), MA Wei-Min(马伟民), WEN Lei (闻雷), et al. Chinese J. Inorg. Chem. (无机化学学报), 2009, 25(5):880-885
18. [18] LI Yu-Ling(李玉玲), MA Wei-Min(马伟民), WEN Lei (闻雷), et al. Acta Metall Sin.(金属学报), 2011, 47(1):95-101[18] LI Yu-Ling(李玉玲), MA Wei-Min(马伟民), WEN Lei (闻雷), et al. Acta Metall Sin.(金属学报), 2011, 47(1):95-101
19. [19] Ji Y M, Jiang D Y, Shi J L. Mater. Lett., 2005, 59:868-871[19] Ji Y M, Jiang D Y, Shi J L. Mater. Lett., 2005, 59:868-871
20. [20] Ji Y M, Jiang D Y, Shi J L. Mater. Res. Bull., 2005, 40:553 -559[20] Ji Y M, Jiang D Y, Shi J L. Mater. Res. Bull., 2005, 40:553 -559
21. [21] RUAN Yan-Li(阮艳莉), TANG Zhi-Yuan(唐致远). Acta Phys. -Chim. Sin. (物理化学学报), 2008, 24(5):873-879[21] RUAN Yan-Li(阮艳莉), TANG Zhi-Yuan(唐致远). Acta Phys. -Chim. Sin. (物理化学学报), 2008, 24(5):873-879
22. [22] ZHU Hong-Yan(朱红艳), MA Wei-Min(马伟民), WEN Lei (闻雷), et al. Acta Metall Sin.(金属学报), 2012, 48(6):671-677[22] ZHU Hong-Yan(朱红艳), MA Wei-Min(马伟民), WEN Lei (闻雷), et al. Acta Metall Sin.(金属学报), 2012, 48(6):671-677
23. [23] TIAN Yan-Wen(田彦文), GAO Hong(高虹), ZHAI Yu-Chun (翟玉春), et al. J. Inorg. Mater. (无机材料学报), 2000, 15 (6):1050-1054[23] TIAN Yan-Wen(田彦文), GAO Hong(高虹), ZHAI Yu-Chun (翟玉春), et al. J. Inorg. Mater. (无机材料学报), 2000, 15 (6):1050-1054
24. [24] ZHOU Hong(周红), ZENG Wen-Ming(曾文明), CHEN Qi-Yuan(陈启元). Chin. J. Nonferrous. Met. (中国有色金属学报), 1993, 3(2):40-43[24] ZHOU Hong(周红), ZENG Wen-Ming(曾文明), CHEN Qi-Yuan(陈启元). Chin. J. Nonferrous. Met. (中国有色金属学报), 1993, 3(2):40-43
25. [25] Guo X, Zhang Z L. Acta Mater., 2003, 51:2539-2547[25] Guo X, Zhang Z L. Acta Mater., 2003, 51:2539-2547

扫一扫看文章

计量

PDF下载量: 0
文章访问数: 1796
HTML全文浏览量: 319

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

正、反向共沉淀法对Pr₂Zr₂O₇纳米粒子表观活化能的影响

通讯作者: 马伟民 maweimin56@163.com

English

Effect of the NSC and RSC Co-precipitation Methods on Apparent Activation Energy of Pr₂Zr₂O₇ Nanopowders

Corresponding author: 马伟民 maweimin56@163.com

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处