Study on purification process of electronic-rade cerium ammonium nitrate through crystallization

doi:10.1016/j.cjche.2025.03.014

Chinese Journal of Chemical Engineering ›› 2025, Vol. 83 ›› Issue (7): 148-159.DOI: 10.1016/j.cjche.2025.03.014

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Study on purification process of electronic-rade cerium ammonium nitrate through crystallization

Yinghan Wang^1,2, Li Yang², Haoliang Wang², Hao Wu³, Jingcai Cheng², Chao Yang^2,4

1 School of Chemical Engineering, University of Jinan, Jinan 250022, China;
2 State Key Laboratory of Petroleum Molecular & Process Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China;
3 Hubei Three Gorges Laboratory, Yichang 443007, China;
4 School of Chemical Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2025-01-09 Revised:2025-03-27 Accepted:2025-03-27 Online:2025-07-28 Published:2025-07-28
Contact: Li Yang,E-mail:yangli@ipe.ac.cn;Jingcai Cheng,E-mail:jccheng@ipe.ac.cn
Supported by:
This research was funded by the National Natural Science Foundation of China (22308358, 22208346, 22421003), IPE Project for Frontier Basic Research (QYJC-2023-05), National Key Research and Development Program (2022YFC3902701), and CAS Project for Young Scientists in Basic Research (YSBR-038).s

Study on purification process of electronic-rade cerium ammonium nitrate through crystallization

Yinghan Wang^1,2, Li Yang², Haoliang Wang², Hao Wu³, Jingcai Cheng², Chao Yang^2,4

1 School of Chemical Engineering, University of Jinan, Jinan 250022, China;
2 State Key Laboratory of Petroleum Molecular & Process Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China;
3 Hubei Three Gorges Laboratory, Yichang 443007, China;
4 School of Chemical Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

通讯作者: Li Yang,E-mail:yangli@ipe.ac.cn;Jingcai Cheng,E-mail:jccheng@ipe.ac.cn
基金资助:
This research was funded by the National Natural Science Foundation of China (22308358, 22208346, 22421003), IPE Project for Frontier Basic Research (QYJC-2023-05), National Key Research and Development Program (2022YFC3902701), and CAS Project for Young Scientists in Basic Research (YSBR-038).s

Abstract

Abstract: The purity of electronic-grade chemicals significantly impacts electronic components. Although crystallization has been used to purify cerium ammonium nitrate (CAN), the impurity removal mechanism underlying different crystallization parameters remains unclear. Traditional analytical methods of inductively coupled plasma mass spectrometry (ICP-MS) have problems in detecting trace Fe accurately, because of the high concentration of Ce and interference of polyatomic ions. Therefore, this study developed a new method integrating the standard addition and internal standard methods and explored the role of the kinetic energy discrimination mode. This new approach effectively overcomes Ce-related matrix interference and fills the gap in ultra-trace impurity detection. Furthermore, the study investigated the effects of cooling rate, seed mass loading and seed size on the removal of Fe impurity. The seed mass loading affects the average crystal size through regulating secondary nucleation and crystal growth. The removal of Fe in CAN is determined by surface adsorption and agglomeration. Under the condition of the cooling rate of 0.2 K·min^-1, and addition of 0.5% (mass) 600-680 mm seeds, the Fe content is the lowest, at only 0.24 mg·L^-1, and the Fe removal rate reaches 92.28%.

Key words: Electronic-grade chemicals, Crystallization, Removal of impurities, ICP-MS, Cerium ammonium nitrate

摘要： The purity of electronic-grade chemicals significantly impacts electronic components. Although crystallization has been used to purify cerium ammonium nitrate (CAN), the impurity removal mechanism underlying different crystallization parameters remains unclear. Traditional analytical methods of inductively coupled plasma mass spectrometry (ICP-MS) have problems in detecting trace Fe accurately, because of the high concentration of Ce and interference of polyatomic ions. Therefore, this study developed a new method integrating the standard addition and internal standard methods and explored the role of the kinetic energy discrimination mode. This new approach effectively overcomes Ce-related matrix interference and fills the gap in ultra-trace impurity detection. Furthermore, the study investigated the effects of cooling rate, seed mass loading and seed size on the removal of Fe impurity. The seed mass loading affects the average crystal size through regulating secondary nucleation and crystal growth. The removal of Fe in CAN is determined by surface adsorption and agglomeration. Under the condition of the cooling rate of 0.2 K·min^-1, and addition of 0.5% (mass) 600-680 mm seeds, the Fe content is the lowest, at only 0.24 mg·L^-1, and the Fe removal rate reaches 92.28%.

关键词: Electronic-grade chemicals, Crystallization, Removal of impurities, ICP-MS, Cerium ammonium nitrate

Yinghan Wang, Li Yang, Haoliang Wang, Hao Wu, Jingcai Cheng, Chao Yang. Study on purification process of electronic-rade cerium ammonium nitrate through crystallization[J]. Chinese Journal of Chemical Engineering, 2025, 83(7): 148-159.

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Study on purification process of electronic-rade cerium ammonium nitrate through crystallization

Study on purification process of electronic-rade cerium ammonium nitrate through crystallization

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