人工晶体学报, 2021, 50 (2): 253, 网络出版: 2021-03-30  

降温速率对DAST单晶生长的影响

Influence of Cooling Rate on the Growth of 4-N,N Dimethylamino-4′-N′-Methyl-Stilbazoliumtosylate (DAST) Single Crystal
孟欢 1,2杨瑞霞 1王健 2,3王增华 2,3马林 1,2
作者单位
1 河北工业大学电子信息工程学院,天津 300401
2 中国电子科技集团有限公司第四十六研究所,天津 300220
3 中国电子科技集团有限公司,新型半导体晶体材料技术重点实验室,天津 300220
摘要
使用籽晶法通过调整降温速率生长出高质量4-N,N-二甲胺基-4′-N′-甲基-氮杂芪对甲苯磺酸盐(DAST)晶体,研究了降温速率对DAST晶体结晶质量、光学特性及太赫兹输出特性的影响。通过核磁共振分析表征了合成原料的结构和纯度。使用X射线衍射仪对生长晶体的(001)面进行X射线摇摆曲线测试,测试结果表明在降温速率为0.1 ℃/d条件下获得的晶体质量最佳,其摇摆曲线半高宽(FWHM)为57.6″。此条件下生长的晶体在780~1 576 nm波长范围内光透过率达65%。使用差频法从DAST晶体中产生了0.1~20 THz范围内的宽频可调谐太赫兹波,在18.8 THz处得到太赫兹波最大输出能量为0.477 μJ/脉冲,对应的能量转换效率达5.31×10-5。
Abstract
High quality 4-N,N-dimethylamino-4′-N′-methyl-stilbazolium tosylate (DAST) crystals were grown by seed crystal method through adjusting cooling rate. The influence of cooling rate on crystal quality, optical properties and terahertz(THz) output characteristics of DAST crystals were explored. Additionally, the structure and purity of raw materials were characterized by applying nuclear magnetic resonance analysis method. X-ray diffraction rocking curve measurement of (001) plane of the as-grown crystals was measured by X-ray diffractometer. A best full-width at half-maximum (FWHM) narrowed as 57.6″ was obtained at the cooling rate of 0.1 ℃/d. Optical transmittance of the crystals grown under these conditions is 65% in the wavelength range of 780 nm to 1 576 nm. Moreover, using the differential frequency method wideband tunable terahertz waves in the range of 0.1 THz to 20 THz were generated from DAST crystals. At 18.8 THz, the maximum output energy of the terahertz wave is 0.477 μJ/pulse, and the corresponding energy conversion efficiency is 5.31×10-5.
参考文献

[1] TAKAHASHI Y, ADACHI H, TANIUCHI T, et al. Organic nonlinear optical DAST crystals for electro-optic measurement and terahertz wave generation[J]. Journal of Photochemistry and Photobiology A: Chemistry, 2006, 183(3): 247-252.

[2] LIU J J, YOU F, HU C, et al. Growth and characterization of organic 4-chlorobenzaldehyde-N- methyl 4-stilbazolium tosylate crystal: a promising material for nonlinear optical device applications[J]. Optik, 2019, 178: 999-1009.

[3] JAGANNATHAN K, KALAINATHAN S, GNANASEKARAN T. Microhardness studies on 4-Dimethylamino-N-methyl 4-Stilbazolium Tosylate (DAST)[J]. Materials Letters, 2007, 61(23/24): 4485-4488.

[4] SUN Z H, CHEN T L, LUO J H, et al. Nucleation kinetics and growth of high-quality DAST crystals with the aid of activated carbon as the adsorbent to micro-crystals in solutions[J]. Journal of Crystal Growth, 2011, 328(1): 89-94.

[5] 徐德刚,朱先立,王与烨,等.基于DAST晶体差频的可调谐THz辐射源[J].光学学报,2020,40(4):0404001.

[6] ADACHI H, TAKAHASHI Y, YABUZAKI J, et al. Growth of high quality nonlinear optical crystal 4-dimethylamino-N-methyl-4-stilbazolium tosylate (DAST)[J]. Journal of Crystal Growth, 1999, 198/199: 568-571.

[7] JAGANNATHAN K, KALAINATHAN S. Growth and characterization of 4-dimethylamino-N-methyl 4-stilbazolium tosylate (DAST) single crystals grown by nucleation reduction method[J]. Materials Research Bulletin, 2007, 42(11): 1881-1887.

[8] HAJA HAMEED A S, YU W C, CHEN Z B, et al. An investigation on the growth and characterization of DAST crystals grown by two zone growth technique[J]. Journal of Crystal Growth, 2005, 282(1/2): 117-124.

[9] SOHMA S, TAKAHASHI H, TANIUCHI T, et al. Organic nonlinear optical crystal DAST growth and its device applications[J]. Chemical Physics, 1999, 245(1/2/3): 359-364.

[10] 马玉哲,钟德高,曹丽凤,等.有机非线性光学晶体DAST及其在太赫兹领域的应用研究进展[J].中国科学:技术科学,2017,47(11):1165-1176.

[11] 孙 箐,滕 冰,曹丽凤,等.DAST晶体的表面形貌、缺陷及显微硬度研究[J].人工晶体学报,2015,44(12):3429-3432.

[12] RUIZ B, JAZBINSEK M, GNTER P. Crystal growth of DAST[J]. Crystal Growth & Design, 2008, 8(11): 4173-4184.

[13] 李 寅,张建秀,傅佩珍,等.有机非线性光学晶体DAST的生长、形貌及透过光谱[J].人工晶体学报,2011,40(1):7-11+16.

[14] CAO L F, TENG B, XU D G, et al. Growth, transmission, Raman spectrum and THz generation of DAST crystal[J]. RSC Advances, 2016, 6(103): 101389-101394.

[15] MORI Y, TAKAHASHI Y, IWAI T, et al. Slope nucleation method for the growth of high-quality 4-dimethylamino-methyl-4-stilbazolium-tosylate (DAST) crystals[J]. Japanese Journal of Applied Physics, 2000, 39(Part 2, No. 10A): L1006-L1008.

[16] ELAHEH G, MAJID J T. The effect of cooling rate on size, quality and morphology of KTiOPO4 (KTP) crystals grown by different nucleation techniques[J]. Crystal Research and Technology, 2015, 50(8): 603-612.

[17] 李德东,江民红,李 林,等.降温速率对无籽固相法生长铌酸钾钠基单晶结构和性能的影响[J].硅酸盐学报,2020,48(9):1446-1454.

[18] PAN F, WONG M S, BOSSHARD C, et al. Crystal growth and characterization of the organic salt 4-N,N-dimethylamino-4′-N-methyl-stilbazolium tosylate (dast)[J]. Advanced Materials, 1996, 8(7): 592-595.

[19] 武 聪,孟大磊,庞子博,等.DAST晶体的生长与表征[J].压电与声光,2017,39(5):722-724.

[20] PANG Z B, MENG D L, XU Y K, et al. Characterization of molecular structure of DAST via NMR spectroscopy[J]. Journal of Molecular Structure, 2016, 1105: 11-15.

[21] CAO L F, TENG B, FENG K, et al. Growth and defects of DAST crystal in high concentration solution[J]. Journal of Crystal Growth, 2015, 412: 20-24.

[22] MARDER S R, PERRY J W, YAKYMYSHYN C P. Organic salts with large second-order optical nonlinearities[J]. Chemistry of Materials, 1994, 6(8): 1137-1147.

[23] KARTHIKEYAN C, HAJA HAMEED A S, SAGAYA AGNES NISHA J, et al. Spectroscopic investigation on the efficient organic nonlinear crystals of pure and diethanolamine added DAST[J]. Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy, 2013, 115: 667-674.

[24] HE Y X, WANG Y Y, XU D G, et al. High-energy and ultra-wideband tunable terahertz source with DAST crystal via difference frequency generation[J]. Applied Physics B, 2017, 124(1): 1-8.

[25] TANIUCHI T, OKADA S, NAKANISHI H. Widely tunable terahertz-wave generation in an organic crystal and its spectroscopic application[J]. Journal of Applied Physics, 2004, 95(11): 5984-5988.

[26] 李 昆,李 春,胡章贵,等.利用国内生长的有机晶体DAST作为THz源的研究[J].光谱学与光谱分析,2006,26(10):1777-1780.

[27] TENG B, WANG S H, FENG K, et al. Crystal growth, quality characterization and THz properties of DAST crystals[J]. Crystal Research and Technology, 2014, 49(12): 943-947.

孟欢, 杨瑞霞, 王健, 王增华, 马林. 降温速率对DAST单晶生长的影响[J]. 人工晶体学报, 2021, 50(2): 253. MENG Huan, YANG Ruixia, WANG Jian, WANG Zenghua, MA Lin. Influence of Cooling Rate on the Growth of 4-N,N Dimethylamino-4′-N′-Methyl-Stilbazoliumtosylate (DAST) Single Crystal[J]. Journal of Synthetic Crystals, 2021, 50(2): 253.

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