添加剂DTPA对KDP晶体快速生长及性能的影响研究

doi:10.3724/SP.J.1077.2012.00405

摘要/Abstract

摘要：

在添加1×10^-4 (mol/mol KDP) 二乙烯三胺五乙酸(DTPA)的溶液中, 利用“点籽晶”快速生长法生长了KDP晶体. 实验发现, 添加少量DTPA即可使不同饱和温度下的KDP生长溶液的亚稳区宽度均得到提高. 利用激光偏振干涉装置研究了不同浓度的DTPA对KDP晶体(100)面生长动力学的影响. 发现随DTPA掺杂量增加, 临界过饱和度(死区)一直降低, 生长速度则是先增加经过一个最大值后减小. 表征了晶体的光学透过率和晶体内部的杂质金属离子含量, 发现掺杂1×10^-4 (mol/mol) DTPA大幅提高了快速生长的KDP晶体在紫外区的透过率, 并有效地减少了进入晶体内部的杂质金属离子含量.

关键词: KDP晶体, 快速生长, 添加剂, 生长动力学, 透过率

Abstract:

KDP crystals were grown by “point seed” rapid growth method in the presence of 1×10^-4 (mol/mol KDP) diethylene triamine penlaacetic acid (DTPA). Metastable zone width of the solutions with different saturation temperatures were extended by adding a small amount of DTPA. The influence of different concentrations of DTPA on the growth kinetics of (100) face of KDP crystal was studied by laser polarization interference technique. With the DTPA concentration increasing, the critical supersaturation (dead zone) was decreased continually, but the growth rate was firstly increased and then decreased, passing through a maximum. The UV-Vis transmission spectra and impurity content of main metal ions in the crystal were characterized as well. The results showed that the optical transmittance in the UV region was enhanced significantly and the impurity content of main metal ions in the crystal was reduced effectively by the addition of 1×10^-4 (mol/mol) DTPA.

Key words: KDP crystal, rapid growth, additive, growth kinetics, optical transmittance

中图分类号:

O781

朱胜军, 王圣来, 丁建旭, 刘光霞, 孙云, 刘文洁. 添加剂DTPA对KDP晶体快速生长及性能的影响研究[J]. 无机材料学报, 2012, 27(4): 405-410.

ZHU Sheng-Jun, WANG Sheng-Lai, DING Jian-Xu, LIU Guang-Xia, SUN Yun, LIU Wen-Jie. Effect of DTPA on Rapid Growth and Performance of KDP Crystal[J]. Journal of Inorganic Materials, 2012, 27(4): 405-410.

图/表 6

图1 纯KDP和掺杂DTPA的KDP溶液的亚稳区宽度

Fig. 1 Metastability limit curves of pure and DTPA-added KDP solution

图2 不同DTPA掺杂浓度下KDP晶体(100)面(a)生长的临界过饱和度和(b)生长速度

Fig. 2 (a) Critical supersaturation of (100) face and (b) dependence of growth rate of (100) face on supersaturation of KDP crystal with different concentrations of DTPA

图3 (a)在未掺杂 DTPA的溶液及(b)掺杂1×10-4 (mol/mol) DTPA的溶液中快速生长的KDP晶体照片

Fig. 3 Photographs of the KDP crystals grown from (a) undoped solution (b) DTPA (1×10-4 mol/mol)-added solution

图4 晶体内部取样位置示意图

Fig. 4 Diagram showing the samples selected in crystal

图5 KDP晶体的透过率曲线

Fig. 5 Transmission spectra of KDP crystals

Table 1 Element result of KDP crystals grown by rapid growth method

Sample number	Dopant concentration of DTPA/ (×10^-6, mol?mol^-1)	Result measured by ICP /(×10^-6, g·g^-1 KDP)
Sample number	Dopant concentration of DTPA/ (×10^-6, mol?mol^-1)	Fe	Cr	Al	Ca	Mg	Na
Raw material of KDP	0	3.160	0.281	2.489	5.891	0.647	14.499
Pyramidal sector	0	1.516	0.253	2.236	3.446	0.625	7.244
Prismatic sector	0	12.073	1.802	14.237	5.199	0.851	16.649
Pyramidal sector	100	0.725	0.140	1.192	2.998	0.490	5.534
Prismatic sector	100	4.219	0.423	6.913	4.557	0.639	7.929

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