原位ATR-IR光谱实时研究DKDP的结晶过程

人工晶体学报 ›› 2022, Vol. 51 ›› Issue (3): 404-410.

原位ATR-IR光谱实时研究DKDP的结晶过程

刘发付^1,2, 张丛¹, 郭建斌¹, 张武¹, 曹剑武¹, 张海波², 徐明霞³

1.内蒙金属材料研究所,包头 014000; 2.华中科技大学材料科学与工程学院,武汉 430073; 3.山东大学晶体材料国家重点实验室,济南 250100

收稿日期:2021-12-09 出版日期:2022-03-15 发布日期:2022-04-11

In Situ ATR-IR Investigation on the Crystallization of DKDP Crystals

LIU Fafu^1,2, ZHANG Cong¹, GUO Jianbin¹, ZHANG Wu¹, CAO Jianwu¹, ZHANG Haibo², XU Mingxia³

1. Inner Mongolia Metal Material Research Institute, Baotou 014000, China;
2. School of Materials Science and Engineering, Huazhong University of Science and Technology, Wuhan 430073, China;
3. State Key Laboratory of Crystal Materials, Shandong University, Jinan 250100, China

Received:2021-12-09 Online:2022-03-15 Published:2022-04-11
Contact: XU Mingxia, doctor, assistant professor. E-mail: mxxu@sdu.edu.cn
About author:LIU Fafu(1988—), male, from Shandong province, doctor, associate researcher. E-mail: fafuliuwyy@163.com
Supported by:
The Elementary Innovation Team Foundation supported by NORINCO Group in China (2021CXTD52); The Taishan Scholars Foundation supported by Shandong Provence in China

摘要/Abstract

摘要： 采用全反模式的红外(ATR-IR)光谱实时研究了不同氘含量KH_2-xD_xPO₄(DKDP)晶体的结晶过程,其中DKDP溶液氘含量范围为0到99%。通过υ₁(PO₄)和υ₃(PO₄)振动表征了DKDP结晶溶液中(H₂PO₄^-)_1-x(D₂PO₄^-)_x离子基团浓度的变化。υ₁(PO₄)振动强度的变化和υ₃(PO₄)振动宽度的变化说明生长溶液中的(H₂PO₄^-)_1-x(D₂PO₄^-)_x离子浓度随着测试时间延长而不断增大。同时,δ(P—O…H/D—O—P)振动峰的形成说明DKDP晶体的生长基元为(H₂PO₄^-)_n-x(D₂PO₄^-)_x离子团簇。波数在1 448 cm^-1到1 653 cm^-1范围内H—O—H和D—O—D振动强度的变化解释了DKDP晶体在结晶过程中氘含量分布不均的现象。

关键词: DKDP单晶, 结晶过程, ATR-IR光谱, (H₂PO₄^-)_n-x(D₂PO₄^-)_x团簇, 氘含量, 生长基元

Abstract: The crystallization of KH_2-xD_xPO₄ (DKDP) crystals with different deuterium contents ranged from 0 to 99% were investigated in solution by Attenuated Total Reflectance Infrared (ATR-IR) spectroscopy. The (H₂PO₄^-)_1-x(D₂PO₄^-)_x ionic groups were characterized by the υ₁(PO₄) and υ₃(PO₄) vibrations. The intensity changes of the υ₁(PO₄) vibration peaks and the broadened width changes of the υ₃(PO₄) vibration peaks indicate that the (H₂PO₄^-)_1-x(D₂PO₄^-)_x concentration increases with the measurement time increases. Besides, the appearance of δ(P—O…H/D—O—P) vibration illustrates the formation of (H₂PO₄^-)_n-x(D₂PO₄^-)_x clusters, which can be confirmed as growth unite.The intensity changes of the H—O—H and D—O—D vibration at the wavenumbers from 1 448 cm^-1 to 1 653 cm^-1can illustrate the un-uniform distribution of deuterium contents in DKDP crystallization process.

Key words: DKDP single crystal, crystallization process, ATR-IR spectroscopy, (H₂PO₄^-)_n-x(D₂PO₄^-)_x clusters, deuterium content, growth unite

刘发付, 张丛, 郭建斌, 张武, 曹剑武, 张海波, 徐明霞. 原位ATR-IR光谱实时研究DKDP的结晶过程[J]. 人工晶体学报, 2022, 51(3): 404-410.

LIU Fafu, ZHANG Cong, GUO Jianbin, ZHANG Wu, CAO Jianwu, ZHANG Haibo, XU Mingxia. In Situ ATR-IR Investigation on the Crystallization of DKDP Crystals[J]. JOURNAL OF SYNTHETIC CRYSTALS, 2022, 51(3): 404-410.

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