Ge-S基玻璃和薄膜二阶非线性光学性能的研究
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摘要
本文为了探索新型二阶非线性光学玻璃材料，采用石英管熔融法制作了Ge-As-S和Ge-Ga-S-Se两个体系的块体硫系玻璃，利用DSC-TG和XRD进行了成玻分析，分析了其紫外-可见光透过率，用Raman谱分析了结构。采用电场／温度场方法进行了极化处理，利用Maker条纹法进行了二阶非线性检测，分析和探讨了硫系玻璃的极化机理，从整体上探索和分析极化工艺及玻璃成分与二阶非线性效应的关系。利用磁控溅射法制备了两个组分的Ge-Ga-S-Se玻璃薄膜。用SEM分析了薄膜的断面形态，在椭偏仪上测得其折射率，并对薄膜进行了Raman光谱、XPS分析，在没有极化的条件下进行了二阶非线性Maker条纹检测。
研究表明：Ge-As-S和Ge-Ga-S-Se体系玻璃的成玻性能非常好，能够制作较大块玻璃，在Ge-As-S体系中短波吸收边随As的增加而向长波方向移动，Ge-S和As-S为玻璃网络形成体。Ge-Ga-S-Se体系中短波吸收边随Se的增加而向长波方向移动，Ge-S，Ga-S，Ge-Se，Ga-Se为玻璃网络形成体。经过极化后两者都产生了明显的Maker条纹。在Ge-As-S体系中随As的增加Maker条纹强度变化不明显。在Ge-Ga-S-Se体系中随着Se含量的增加，Maker条纹强度明显增加。这说明Se的加入有利于二阶非线性效应的增强。
用磁控溅射方法以此靶材溅射得到了1-10μm厚的、均匀的Ge-Ga-S-Se硫系玻璃薄膜，其大的折射率表明其用于集成光学具有明显的优势。利用S和Se溅射速率的不同，通过调制溅射条件可以在同一靶材上制得不同的组分、从而得到不同折射率的玻璃薄膜，可以很方便地用于光波导技术。该薄膜不用极化处理，就产生了显著的Maker条纹。结果表明薄膜的制备方法影响了薄膜的微观结构，磁控溅射过程中，电场和磁场影响了靶材原子的沉积，使玻璃薄膜中的电偶极子在一定程度上得到了定向排布，使薄膜呈现出显著的二阶非线性效应。
For the purpose to exploit new type of second order non-linear optic glasses, Ge-As-S and Ge-Ga-S-S bulk chalcogenide glasses were prepared by traditional quench method. DSC-TG and XRD were utilized to analyze the glass-forming ability of these glasses. Transmission was done on UV-Visible Spectrophotometer. Raman spectroscopy was used to analyze the structure. Ge-Ga-S-S glass films were deposited by RF magneto sputtering. SEM was used to observe the surface and the cross section of the films. Index of refractive was derived from the ellipsometer. Raman spectroscopy and XPS were used to analyze the structure and composition of the films.
Homogeneous bulk glasses of Ge-As-S and Ge-Ga-S-Se could be easily prepared. In the Ge-As-S system the UV absorption edge shifted towards the longer wavelength with the increase of As content, while in the Ge-Ga-S-Se system, with the increase of Se. And in Ge-As-S system, Ge-S and As-S were the glass formers, while in Ge-Ga-S-Se, Ge-S, Ga-S, Ge-Se, Ga-Se were the glass formers. Having been Thermally/Electrically poled, the SHG maker fringes were obviously observed. In Ge-Ga-S-Se the SHG intensity changed appreciably with the increase of Se content. Bipolar alignment model was adopted to interpret for the generation of SHG.
Homogeneous films were deposited from l-10um in thickness. The compositions varied with different sputtering power and the type of the elements. XRD analysis proved that the films were still amorphous. Raman analysis indicated that the composition and structure varied from the bulk glasses in that the sputtering rate for each element was different. More Se-Se bonds formed in the films. The SHG was found in as-prepared films and the intensity of film with 20% Se was bigger then that of 10% Se films. This phenomenon indicated that the film had been poled during the fabrication, due to the influence of electric field and magnetic field.
研究表明：Ge-As-S和Ge-Ga-S-Se体系玻璃的成玻性能非常好，能够制作较大块玻璃，在Ge-As-S体系中短波吸收边随As的增加而向长波方向移动，Ge-S和As-S为玻璃网络形成体。Ge-Ga-S-Se体系中短波吸收边随Se的增加而向长波方向移动，Ge-S，Ga-S，Ge-Se，Ga-Se为玻璃网络形成体。经过极化后两者都产生了明显的Maker条纹。在Ge-As-S体系中随As的增加Maker条纹强度变化不明显。在Ge-Ga-S-Se体系中随着Se含量的增加，Maker条纹强度明显增加。这说明Se的加入有利于二阶非线性效应的增强。
用磁控溅射方法以此靶材溅射得到了1-10μm厚的、均匀的Ge-Ga-S-Se硫系玻璃薄膜，其大的折射率表明其用于集成光学具有明显的优势。利用S和Se溅射速率的不同，通过调制溅射条件可以在同一靶材上制得不同的组分、从而得到不同折射率的玻璃薄膜，可以很方便地用于光波导技术。该薄膜不用极化处理，就产生了显著的Maker条纹。结果表明薄膜的制备方法影响了薄膜的微观结构，磁控溅射过程中，电场和磁场影响了靶材原子的沉积，使玻璃薄膜中的电偶极子在一定程度上得到了定向排布，使薄膜呈现出显著的二阶非线性效应。
For the purpose to exploit new type of second order non-linear optic glasses, Ge-As-S and Ge-Ga-S-S bulk chalcogenide glasses were prepared by traditional quench method. DSC-TG and XRD were utilized to analyze the glass-forming ability of these glasses. Transmission was done on UV-Visible Spectrophotometer. Raman spectroscopy was used to analyze the structure. Ge-Ga-S-S glass films were deposited by RF magneto sputtering. SEM was used to observe the surface and the cross section of the films. Index of refractive was derived from the ellipsometer. Raman spectroscopy and XPS were used to analyze the structure and composition of the films.
Homogeneous bulk glasses of Ge-As-S and Ge-Ga-S-Se could be easily prepared. In the Ge-As-S system the UV absorption edge shifted towards the longer wavelength with the increase of As content, while in the Ge-Ga-S-Se system, with the increase of Se. And in Ge-As-S system, Ge-S and As-S were the glass formers, while in Ge-Ga-S-Se, Ge-S, Ga-S, Ge-Se, Ga-Se were the glass formers. Having been Thermally/Electrically poled, the SHG maker fringes were obviously observed. In Ge-Ga-S-Se the SHG intensity changed appreciably with the increase of Se content. Bipolar alignment model was adopted to interpret for the generation of SHG.
Homogeneous films were deposited from l-10um in thickness. The compositions varied with different sputtering power and the type of the elements. XRD analysis proved that the films were still amorphous. Raman analysis indicated that the composition and structure varied from the bulk glasses in that the sputtering rate for each element was different. More Se-Se bonds formed in the films. The SHG was found in as-prepared films and the intensity of film with 20% Se was bigger then that of 10% Se films. This phenomenon indicated that the film had been poled during the fabrication, due to the influence of electric field and magnetic field.
引文
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[10] 杨尊先，若干氧化物玻璃性能与结构研究，武汉理工大学硕士学位论文，武汉：武汉理工大学，2001
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[13] 洪海平，王业斌，林绮，周淑琴，金祥风，无机非线性光学材料的探索，化学通报，1994，10，65-68
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[15] R.A.Myer, N.Mukherjee and S.R.J.Large second-order nonlinearity in poled fused silica,Opt.Lett., 1991 ,16(22), 1732-1734
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[18] 孙小函，硅酸盐学报，1994，22(5)，434-437
[19] 泉谷彻郎著，杨淑清 译，光学玻璃与激光玻璃开发，北京：兵器工业出版社 1996
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[21] N.Mukherjee,R.A.Myers,and S.R.Brueck, Dynamic of second-harmonic generation in fused silica,J.Opt.Soc.Am.B,1994,242,665-669
[22] H.Nasu ,K.Kurachi, K.Kamiya,A.Mito, Second harmonic generation from bulk silica and silicate glasses, J.Non-Cryst.Solids, 178,1994,23
[23] H.Nasu, K.Kurachi,H.Okamoto,J.Matsuoka, K.Kamiya,A.Mito, Second harmonic generation from an electrically polarized TiO_2-containing silicate glass,J. Non-Cryst. Solids., 32,1993,83-86
[24] Z.Xu,L.Liu,Z.Hou ,Influence of different poling method on second-order nonlinearity in fused silica glasses, Opt.Comm, 2000, 174, 675-479
[25] K.Tanaka , K.Kamiya,K.Hirao,N.Soga., A.Mito,H.Nasu Second harmonic generation in the electrically poled Li_2O-Nb_2O_5-TeO_2 glasses, J.Non-cryst.,Solids., 1995,185,123-126
[26] K.Tanaka, Y.Yamamoto,H.Nasu,T.Hashimoto,K.Kamiya Optical second harmonic generation in poled MgO-ZnO-TeO_2 an BeO3-TeO2 glasses, J.Non-Cryst.Solids, 1996,203,49-54
[27] A.Mito,U.Tsukuba,H.Nasu, Second harmonic generation in electrically poled TeO2-based glasses, SPIE. 1994, 2289, 167-176
[28] 陈红兵，徐建华，余保龙，朱从善，陆兴泽，干福熹，电极化条件 对石英玻璃德电致二阶非线性光学效应德影响 中国激光，1998，25(1)，56-60
[29] H.Chen,H,Xia,C.Zhu and F, Gan,Second harmonic generation from electrically polarized CuCl-microcrystallite-doped glasses, J.Non-Cryst.Solids, 50, 2001, 333-336
[30] H.Chen,C.Zhau.B.Yu and F.Gan,Preparation and optical properties of Cul micro-crystallite-doped borosilicate glasses,J.Non-Cryst.Solids, 262, 2000,282-286
[31] Y.Yamato,H.Nasu,T.Hashimoto,K.Kamiya .,Second harmonic generation from thermally poled CdS microcrystal-containing glasses. J.Non-Cryst.Solids, 2001, 281, 198-204
[32] 刘启明，赵修建，干福熹，电子束辐照下Ge-As—S硫系玻璃的二阶非线性光学效效应，光学学报。2001，21(6)，683—686
[33] 刘启明，赵修建，干福熹，Ge-As-S体系玻璃中光学二次谐波发生及其极化机理分析，物理学报，49(9)，2000，1726—173
[34] Q,M.Liu,X.J.Zhao, K.Tanaka.,A.Narazaki,K.Hirao,F.X.Gan,Second harmonic generation in Ge-As-S glasses by electronic beam irradiation analysis of the poled mechanism,Opt.commun, 198, 2001, 187-192
[35] D.S.Chemla, Phys. Rev., 1975, B12, 4534-4537
[36] C.T.Chen，物理学报，1976，25，146：中国科学报，1979，22，756-759
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