CdSiP2晶体中光散射颗粒的研究

doi:10.15541/jim20130601

无机材料学报 ›› 2014, Vol. 29 ›› Issue (8): 855-858.DOI: 10.15541/jim20130601

CdSiP₂晶体中光散射颗粒的研究

张国栋, 李春龙, 王善朋, 张翔, 张西霞, 陶绪堂

(山东大学晶体材料国家重点实验室山东大学晶体材料研究所, 济南 250100)

收稿日期:2013-11-18 修回日期:2013-12-31 出版日期:2014-08-20 网络出版日期:2014-07-15
作者简介:张国栋(1981–), 男, 博士. E-mail: zhguodong@126.com
基金资助:
国家自然科学基金(51272129;50721002;50990061;50802054);国家重点基础研究发展计划项目(“973”)(2010CB 630702)

Investigations on Optical Scatter Particles during CdSiP₂ Crystals Growth

ZHANG Guo-Dong, LI Chun-Long, WANG Shan-Peng, ZHANG Xiang, ZHANG Xi-Xia, TAO Xu-Tang

(State Key Laboratory of Crystal Materials, Institute of Crystal Materials, Shandong University, Jinan 250100, China)

Received:2013-11-18 Revised:2013-12-31 Published:2014-08-20 Online:2014-07-15
About author:ZHANG Guo-Dong. E-mail: zhguodong@126.com
Supported by:
National Natural Science Foundation of China (51272129;50721002;50990061;50802054);National Basic Research Program of China (2010CB630702)

摘要/Abstract

摘要：

采用单温区法合成了CdSiP₂ (CSP)多晶原料, 然后采用垂直布里奇曼法生长了大尺寸的CSP单晶。采用扫描电子显微镜、EDS对晶体中光散射颗粒的尺寸、形貌和成分进行了观察和检测。测试结果表明, 所生长的CSP晶体中的光散射颗粒呈近椭圆形, 尺寸为2~8 μm, 主要成分为Si, 含量占88%以上。对CSP多晶合成的反应机理研究表明, 此第二相颗粒是由于合成时多晶料中残留有少量未反应的Si单质所致。通过合成工艺的改进, 有效地减少了晶体中Si散射颗粒的残留, 制备出了高透明性的CSP单晶体。

关键词: 磷硅镉, 非线性光学晶体, 晶体缺陷, 垂直布里奇曼法

Abstract:

Polycrystalline charges of CdSiP₂ (CSP) were synthesized by direct reaction method using P, Si, and Cd elements as the initial materials. Single crystals with the dimension of 8 mm in diameter and 40 mm in length were successfully grown by vertical Bridgman method. The dimension and the composition of the optical scatter particles in the CSP crystals were identified by SEM measurement. The results show that most of optical scattering particles are round-shaped with dimension of 2-8 μm. The EDS measurement result shows that the atomic percent of Si in the optical scattering particles is over 88%. The synthesis mechanism of CSP by single temperature zone method was studied by powder XRD. The results show that there is some unreacted silicon left when synthsized process is carried out below 1150℃. By optimizing the synthesis parameters and the Si inclusions were successfully restrained and the high optical quality CSP single crystal was obtained.

Key words: CdSiP2, nonlinear optical crystal, crystal defect, vertical Bridgman growth

中图分类号:

O782

张国栋, 李春龙, 王善朋, 张翔, 张西霞, 陶绪堂. CdSiP₂晶体中光散射颗粒的研究[J]. 无机材料学报, 2014, 29(8): 855-858.

ZHANG Guo-Dong, LI Chun-Long, WANG Shan-Peng, ZHANG Xiang, ZHANG Xi-Xia, TAO Xu-Tang. Investigations on Optical Scatter Particles during CdSiP₂ Crystals Growth[J]. Journal of Inorganic Materials, 2014, 29(8): 855-858.

图/表 6

图1 抛光后的CSP晶体照片

Fig. 1 Photograph of polished CSP single crystal

图2 晶体中散射颗粒的SEM照片

Fig. 2 SEM image of the inclusions in CSP crystal

表1 CSP晶体内夹杂相与透明相的成分

Table 1 Compositions of inclusions and CSP “clear area” measured by EDS

Element	Scatter particles		CSP
Element	wt%	at%	wt%	at%
Si	79.28	88.23	13.02	23.30
P	8.23	8.30	32.17	52.19
Cd	12.49	3.47	54.81	24.51
Total	100.00	100.00	100.00	100.00

图3 不同合成温度下产物的粉末XRD图谱

Fig. 3 Powder XRD patterns of the products reacted at different temperatures (a) 500℃; (b) 600℃; (c) 700℃; (d1) 780℃ (products at the top of the ample); (d2) 780℃ (products at the bottom of the ample); (e) 1050℃; (f) 1150℃

图4 具有散射颗粒(a)和无散射颗粒(b)CSP晶体的透过光谱

Fig. 4 Transmission spectra of CSP crystal with inclusions and (a) inclusions-free CSP crystal (b)

图5 高质量的CSP晶体的照片

Fig. 5 High quality CSP single crystal without optical scattering particles

参考文献 17

[1]	ZHANG GUO-DONG, WANG SHAN-PENG, TAO XU-TANG. Research progress of infrared nonlinear optical crystals. Journal of Synthetic Crystals. 2012, 41: 17-23.
[2]	PETROV V. Parametric down-conversion devices: The coverage of the mid-infrared spectral range by solid-state laser sources .Optical Materials, 2012, 34: 536-554.
[3]	ZAWILSKI K T, SCHUNEMANN P G, POLLAK T C, et al. Growth and characterization of large CdSiP2 single crystals .Journal of Crystal Growth, 2010, 312: 1127-1132.
[4]	PETROV V, NOACK F, TUNCHEV I, et al. The nonlinear coefficient d36 of CdSiP2. Proc. of SPIE, 2009, 7197: 71970M-1.
[5]	BORSHCHEVSKII A S, GORYUNOVA N A, KESAMANLY F P, et al. Semiconducting AⅡBⅣCⅤ2 compounds. Phys. Status Solidi, 1967, 21(1): 9-55.
[6]	Spring-Thorpe A J, Pamplin B R. Growth of some single crystal II-IV-V2 semiconducting compounds. Journal of Crystal Growth, 1968, 3-4: 313-316.
[7]	KATO K, UMEMURA N, PETROV V. Sellmeier and thermo-optic dispersion formulas for CdSiP2. Journal of Applied Physics, 2011, 109(11): 116104-1-2.
[8]	KEMLIN V, BRAND P, BOULANGER B. Phase-matching properties and refined Sellmeier equations of the new nonlinear infrared crystal CdSiP2. Optical Letters, 2011, 36(10): 1800-1802.
[9]	ANDRE PEREMANS, DAN LIS, FRANCESCA CECCHET, et al. Noncritical singly resonant synchronously pumped OPO for generation of picosecond pulses in the mid-infrared near 6.4 μm .Optics Letters, 2009, 34(20): 3053-3055.
[10]	PETROV V, SCHUNEMANN P G, ZAWILSKI K T, et al. Noncritical singly resonant optical parametric oscillator operation near 6.2 μm based on a CdSiP2 crystal pumped at 1064 nm. Optics Letters, 2009, 34(16): 2399-2401.
[11]	CHALUS O, SCHUNEMANN PG, ZAWILSKI K F, et al. Optical parametric generation in CdSiP2. Optics Letters, 2010, 35(24): 4142-4144.
[12]	MARCHEV G, TYAZHEV A, PETROV V, et al. Optical parametric generation in CdSiP2 at 6.125 μm pumped by 8 ns long pulses at 1064 nm. Optics Letters, 2012, 37(4): 740-742.
[13]	ZHANG GUO-DONG, TAO XU-TANG, RUAN HUA-PENG, et al. Growth of CdSiP2 single crystals by self-seeding vertical Bridgman method. Journal of Crystal Growth, 2012, 340(1): 197-201.
[14]	ZHANG GUO-DONG, RUAN HUA-PENG, ZHANG XIANG, et al. Vertical Bridgman growth and optical properties of CdSiP2 crystals. CrystEngComm., 2013, 15(21): 4255-4260.
[15]	LIU CUN-YI. Synthesis of and diffusion of Cd in InP .Semiconductor Optoelectronics. 1982, 4: 5-7.
[16]	LIU GUANG-YAO, ZHU SHI-FU, ZHAO BEI-JUN, et al. Technological studies on explosion-proof of CdSiP2 polycrystalline synthesis .Journal of Synthetic Crystals, 2012, 41(6): 1483-1487.
[17]	戴永年.二元合金相图集.上海: 科学出版社, 2009: 293.

CdSiP₂晶体中光散射颗粒的研究

Investigations on Optical Scatter Particles during CdSiP₂ Crystals Growth

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