CN112323145B - 红外非线性光学晶体KAg3Ga8Se14及其制备方法和用途 - Google Patents
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Abstract
本发明涉及一种红外非线性光学晶体KAg3Ga8Se14及其制备方法和用途。该晶体的化学式为KAg3Ga8Se14,分子量为2025.91,结晶于非中心对称的单斜晶系空间群Cm,其晶胞参数为:a=12.8805(5) Å,b=11.6857(4) Å,c=9.6600(4) Å,α=γ=90°,β=115.9980(1)°,Z=2,单胞体积为1306.87(9) Å3。本发明提供的KAg3Ga8Se14晶体具有倍频效应高、抗激光损伤阈值高、红外透过范围宽、空气中稳定等优点,是一种新的红外非线性光学晶体材料,可作为近红外非线性光学晶体在全固态激光器中获得应用。
Description
技术领域
本发明属于非线性光学晶体技术领域,特别涉及一种二阶非线性光学晶体及制备方法和作为非线性光学器件的用途。
背景技术
非线性光学(NLO)晶体作为一类基于激光技术应用上的新型功能材料,具有倍频、和频、差频、参量放大等效应,只有无对称中心的晶体才具备非线性光学效应,而这种非线性光学晶体是通过激光频率转换以获得更多波长的不可或缺的部件。被制成二次谐波发生器,上、下频率转换器,光参量振荡器等器件,可应用于激光武器、激光存储、通讯传感等重要领域。
当前紫外、可见-近红外波段的非线性光学晶体已经可以满足实际应用的需求;如在二倍频(532 nm)的晶体主要有LBO(LiB3O5)、BBO(β-BaB2O4)、KTP(KTiOPO4);在三倍频(355nm)晶体有BBO、LBO、CBO(CsB3O5)。与之相比,在红外波段的非线性光学晶体发展还很缓慢。包括黄铜矿结构的AGS(AgGaS2)和ZGP(ZnGeP2)等较为成功的红外非线性光学晶体存在着严重的缺陷,限制了它们的应用。因此,探寻具有综合性能优良的新型红外非线性光学晶体以满足应用是十分必要的。
发明内容
本发明的目的在于提供一种KAg3Ga8Se14非线性光学晶体。
本发明的另一目的在于提供KAg3Ga8Se14非线性光学晶体的制备方法。
本发明的再一目的在于提供KAg3Ga8Se14非线性光学晶体的用途。
实现本发明目的的技术解决方案如下:
本发明提供的KAg3Ga8Se14非线性光学晶体,该KAg3Ga8Se14非线性光学晶体不具备对称中心,属于单斜晶系,空间群为Cm,其晶胞参数为:a = 12.8805(5) Å, b = 11.6857(4) Å, c = 9.6600(4) Å, α = γ = 90°, β = 115.9980(1)°, Z = 2, 单胞体积为1306.87(9) Å3,分子量为2025.91。
本发明KAg3Ga8Se14非线性光学晶体的制备方法,采用高温固相合成法,具体包括如下步骤:将Ag源材料、Ga源材料、Se单质按照Ag:Ga:Se = 3:8:14的摩尔比投料,加入过量的碘化钾作为K源以及助熔剂,混合研磨后压片,然后用火焰密封于抽真空的石英管中,在800~1000 ℃下反应24小时以上,然后以3~6 ℃/小时的降温速度缓慢降温至400 ℃或以下,得到含有橙色KAg3Ga8Se14晶体的产物,使用蒸馏水或无水乙醇洗涤产物,经超声波处理分离,干燥后得到KAg3Ga8Se14晶体。
较佳的,所述Ag源材料为Ag单质或氧化银(Ag2O);
较佳的,所述Ga源材料为Ga单质或氧化镓(Ga2O3)。
较佳的,当Ag源材料、Ga源材料为氧化物时,加入B:O = 2:3的B单质作为还原剂。
本发明提供了KAg3Ga8Se14非线性光学晶体的用途,该KAg3Ga8Se14非线性光学晶体可用于制备非线性光学器件。
优选的,所述非线性光学器件包含将至少一束入射电磁辐射通过所述KAg3Ga8Se14非线性光学晶体后产生至少一束频率不同于所述入射电磁辐射的输出辐射的装置。
与现有技术相比,本发明的优点是:
本发明所述的KAg3Ga8Se14非线性光学晶体的合成方法简单、易操作、原料易得、可重复性好,且容易得到较大尺寸的晶体。
本发明所述的KAg3Ga8Se14非线性光学晶体具有稳定的物理化学性质,不易碎裂,不易潮解,在空气中可长时间稳定存在。
粉末红外倍频实验表明,KAg3Ga8Se14具有较为良好的红外非线性光学性能,在2.1μm激光照射下,有较强的倍频光输出,其粉末(粒度210-250 μm)SHG强度约为相应粒度AgGaS2的0.6倍。
附图说明
图1是本发明涉及的化合物KAg3Ga8Se14的晶体结构图。
图2是本发明涉及的化合物KAg3Ga8Se14非线性光学晶体的纯相粉末X射线衍射图。
图3是本发明涉及的化合物KAg3Ga8Se14非线性光学晶体SHG强度对比图。
图4是本发明涉及的化合物KAg3Ga8Se14非线性光学晶体的相位匹配图。
具体实施方式
本发明通过以下实施例进行详细说明。但下述实施例不是对本发明保护范围的限制。任何在本发明基础上做出的改进和变化,都在本发明的保护范围之内。
实施例
按照Ag:Ga:Se =3:8:14元素摩尔比称量Ag2O、Ga2O3和Se,加入过量的碘化钾作为K源以及助熔剂,加入与Ag2O、Ga2O3中的氧元素相应摩尔比(B:O = 2:3)的B单质作为还原剂。混合研磨后压片,然后用火焰密封于抽真空的石英管中,在950 ℃下反应24小时以上,然后以5 ℃/小时的降温速度缓慢降温至300 ℃,得到含有橙色KAg3Ga8Se14晶体的产物,使用蒸馏水或无水乙醇洗涤产物,经超声波处理分离,干燥后得到KAg3Ga8Se14晶体。通过单晶X射线衍射分析,表明该化合物为KAg3Ga8Se14,晶体参数如下:
该化合物的单胞参数为:a = 12.8805(5) Å, b = 11.6857(4) Å, c = 9.6600(4) Å, α = γ = 90°, β = 115.9980(1)°, Z = 2。分子量为2026.4,属于单斜晶系,空间群为Cm。结构如附图1所示。
将所制备的KAg3Ga8Se14晶体使用玛瑙研钵研磨多次后,对所得KAg3Ga8Se14粉末进行粉末X射线衍射分析,结果参见图2。从图2中看出,实验值与理论值吻合,说明得到的粉末样品为纯相。
图3是该实施例中的化合物KAg3Ga8Se14非线性光学晶体SHG强度对比图,在实验测定其粉末(粒度210-250 μm)SHG强度约为相应粒度AgGaS2的0.6倍。
图4是该实施例中的化合物KAg3Ga8Se14非线性光学晶体的相位匹配图,从图4中可以看出其满足相位匹配。
Claims (7)
1.一种红外非线性光学晶体,其特征在于,它的化学式为KAg3Ga8Se14,分子量为2025.91,结晶于非中心对称的单斜晶系空间群Cm,其晶胞参数为:a = 12.8805(5) Å, b =11.6857(4) Å, c = 9.6600(4) Å, α = γ = 90°, β = 115.9980(1)°, Z = 2, 单胞体积为1306.87(9) Å3。
2. 一种红外非线性光学晶体的制备方法,其特征在于,采用高温固相合成法,具体包括如下步骤:将Ag源材料、Ga源材料、Se单质按照Ag:Ga:Se = 3:8:14的摩尔比投料,加入过量的碘化钾作为K源以及助熔剂,混合研磨后压片,然后用火焰密封于抽真空的石英管中,在800~1000 ℃下反应24小时以上,然后以3~6 ℃/小时的降温速度缓慢降温至400 ℃或以下,得到含有橙色KAg3Ga8Se14晶体的产物,使用蒸馏水或无水乙醇洗涤产物,经超声波处理分离,干燥后得到KAg3Ga8Se14晶体。
3.如权利要求2所述的方法,其特征在于,所述Ag源材料为Ag单质或氧化银。
4.如权利要求2所述的方法,其特征在于,所述Ga源材料为Ga单质或氧化镓。
5. 如权利要求2所述的方法,其特征在于,所述Ag源材料为Ag2O,所述Ga源材料为Ga2O3,加入与Ag2O、Ga2O3中的氧元素相应摩尔比即B:O = 2:3的B单质作为还原剂。
6.如权利要求1所述的红外非线性光学晶体在制备非线性光学器件中的用途。
7.如权利要求6所述的用途,其特征在于,所述非线性光学器件包含将至少一束入射电磁辐射通过所述红外非线性光学晶体后产生至少一束频率不同于所述入射电磁辐射的输出辐射的装置。
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CN107399722A (zh) * | 2017-08-15 | 2017-11-28 | 中国科学院新疆理化技术研究所 | 硒硅银钡和硒硅银钡中远红外非线性光学晶体及制备方法和用途 |
CN110777434A (zh) * | 2019-11-12 | 2020-02-11 | 中国工程物理研究院化工材料研究所 | 一种混合阴离子红外非线性光学晶体/粉末及其制备方法 |
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