CN112110649A - 一种碲铋酸盐中红外2.7微米发光玻璃及其制备方法 - Google Patents
一种碲铋酸盐中红外2.7微米发光玻璃及其制备方法 Download PDFInfo
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- -1 tellurium bismuth salt Chemical class 0.000 description 1
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Abstract
本发明公开了一种掺铒碲铋酸盐中红外2.7微米发光玻璃,其组分包括:TeO2,Bi2O3,ZnO,ZnCl2,Na2O,ErCl3。通过熔融法制得的玻璃,具有良好的机械性能,获得了Er离子在2700附近的发光,是一种非常有前景的高光学质量玻璃;利用重金属氧化物及卤族元素改善玻璃机械性能和提升玻璃红外发光性能,制备方法简便,制备周期短,有望应用于国防工业、军事及民用领域。
Description
技术领域
本发明涉及一种掺铒碲铋酸盐中红外玻璃及其制备方法。
背景技术
中红外2~5μm波段稀土掺杂激光玻璃及光纤在国家安全与国防建设、光通信、天体物理探测与光谱学研究等领域都将具有广泛的应用前景。在整个中红外光谱中,中红外~3μm波段由于更接近O-H键基本伸缩振动频率,水分子对于~3μm激光吸收系数远远高于其他波段,研究表明,水对Er3+:YSGG 2.8μm激光的吸收是Ho3+:YAG 2.1μm激光的200倍,是Nd3+:YAG 1.06μm激光的10000倍。~3μm激光对生物组织的作用几乎观察不到碳化,并且消融速度相对更快,对相邻组织具有最小的热扩散和机械损伤,能够用于软组织的精确切割,因此,~3μm波段的激光被称为皮肤病学,外科手术和牙科领域的“黄金激光”。尽管如此,此类激光设备目前并没有得到完全的商业化,仍然只是停留在实验阶段,开发高功率3μm激光器尤其是光纤激光器将有极大的潜力革新医学领域。另外由于大气组成中许多重要的气体分子如CO2,H2O,CO,N2O等的主要吸收峰都在~3μm波段,红外乃至中红外波段高功率可调谐超短脉冲激光作为非线性激光雷达也已成为目前大气环境监测领域的研究热点,由于~3μm波段具有对相应大气分子的识别能力,以此可以实时监测大气的组成,获得大气云图,气象变化等信息,相比于传统的探测方式,使用激光探测的方式更加简单便捷。基于此,~3μm波段激光在整个中红外波段光源中占据了重要的地位,开发~3μm波段激光器件将极大的推动科技与人类文明的进步。
目前,仅在掺铒氟化物玻璃中获得3μm激光输出,但是氟化物玻璃因其固有的缺陷,化学稳定性和机械强度较差、制备条件苛刻、易被水分侵蚀、抗析晶性能差(ΔT≤85℃)等限制了其激光功率的提高。硅酸盐玻璃声子能量高(~1100cm~1),稀土无辐射跃迁几率高,不利于获得高效发光。亟需发展一种声子能量低,热稳定性能优良的新型2μm波段掺铒玻璃体系。碲酸盐玻璃的声子能量较低(700~750cm~1),有利于提高稀土辐射跃迁几率,发光效率较高。但是碲酸盐玻璃也存在热稳定性能、机械性能较差的问题,可通过在碲酸盐玻璃中添加适量重金属氧化物替代一部分氧化碲作为玻璃形成体,形成碲铋酸盐玻璃,改善玻璃的热稳定性能和机械性能。
为了进一步改善玻璃的各项性能,在玻璃中引入重金属氯化物使得玻璃网络结构中形成[ZnCl4]空间四面体。由于它具有更低的声子能量(200~300cm-1)并且均匀的分布在玻璃网络结构中使得声子能量进一步降低,提升中红外的发光性能。
发明内容
本发明的目的在于提供一种掺铒碲铋酸盐中红外玻璃及其制备方法。与以往的玻璃基质材料相比,该种材料克服了碲酸盐玻璃(较差的热稳定性)所固有的缺点,在提高玻璃热稳定性和机械强度的基础上,在980nm波长的激光二极管泵浦下同时获得很强的2.7μm荧光,为中红外波段激光器提供一种合适的基质材料。
本发明具体的技术解决方案如下:
一种掺铥碲锗酸盐中红外玻璃:以TeO2为主要组分,摩尔百分比组成包括:TeO2:50~65%,Bi2O3:5%~10%,ZnO:0~15%,ZnCl2:0~30%,Na2O:10%,ErCl3:1%。
所述的掺铒碲铋酸盐中红外玻璃,包括下列步骤:
(1)制备技术:按照玻璃组成的摩尔百分比,计算出相应各组成的重量,称取原料;所有原料组分研磨均匀形成混合料后,放入铂金坩埚中,并置于750~800℃的硅碳棒电炉中熔制20~30分钟,均化和澄清后得到均匀无气泡的玻璃液;
进一步地,在步骤(1)的熔制过程中以搅拌的形式使铂金坩埚中混合均匀排除气泡;
(2)浇注:将步骤(2)得到的玻璃液快速浇注到已预热至300~350℃的模具上;
(3)退火:后再放入已升温至250~300℃的马弗炉中,保温2~3小时后,然后关闭马弗炉,降温至室温。
本发明的有益效果:
(1)在碲酸盐玻璃中引入Bi2O3,机械性能得到显著地提高;
(2)在碲酸盐玻璃中引入ZnCl2,ZnCl2的加入可以提高玻璃的硬度和热稳定性,当ZnCl2加入达到20mol%,玻璃网络中形成[ZnCl4]四面体结构单元。因此氯化锌的加入量需大于20mol%使得2.7μm处的荧光强度突增。同时能够提供具有低Tg而又具有更大的ΔT(Tx-Tg)的玻璃;
(3)该碲酸盐玻璃熔制温度低,并且玻璃转变温度低,具有良好的热稳定性能,制作工艺简单,绿色环保,生产成本也较低,容易制备获得高光学质量玻璃;
(4)在980nm半导体激光器的泵浦下,本发明实施例所得含铒碲铋酸盐玻璃在2500~3000nm范围内可获得较强的中心波长在2.7μm的发光,基于Er3+:4I13/2→4I15/2能级之间的辐射跃迁;
(5)在650nm半导体激光器的泵浦下,本发明实施例所得含铒碲铋酸盐玻璃在2500~3000nm范围内可获得强的中心波长在2.7μm的发光,基于Er3+:4I13/2→4I15/2能级之间的辐射跃迁。
附图说明
图1为实施例2中样品2-8#掺铒碲铋酸盐玻璃在980nm波长的激光二极管泵浦下发光图谱。图2为实施例2中样品2-8#掺铒碲铋酸盐玻璃在650nm波长的激光二极管泵浦下发光图谱。
具体实施方式
以下具体实施例对本发明作示例性的说明及帮助进一步理解本发明,但实施案例具体细节仅是为了说明本发明,并不代表本发明构思下全部的技术方案,因此不应理解为对本发明总的技术方案的限定,一些在技术人员看来,不偏离本发明构思的非实质性增加和改动,例如以具有相同或相似技术效果的技术特征简单改换或替换,均属于本发明保护范围。
表1:
实施例1
一种碲酸盐玻璃,原料组成如表1中1-2#所示;
按照表1中1-2#玻璃组成的质量百分比,计算出相应的各组成的重量,并称取各原料组分;将原料研磨均匀形成混合料后,放入铂金坩埚中,并置于750~800℃的硅碳棒电炉中熔制20分钟得到熔融的玻璃液,在玻璃熔制过程中始终通入高纯氧气进行气氛保护以除去玻璃液中的水分。除去水分的玻璃液经均化澄清,然后快速浇注到已预热至300~350℃的模具上,后再放入已升温至所述玻璃液的250~300℃的马弗炉中,保温3小时后,然后关闭马弗炉,降温至室温,完全冷却后取出玻璃样品。
对玻璃的测试结果如下:
①对制备的两块玻璃通过经典的应力应变法进行三点弯曲强度测试,测试结果表示当Bi2O3掺杂浓度为10mol%时,玻璃的三点弯曲强度从40MPa提升至62.35MPa.较好的机械性能提高了碲铋酸盐玻璃作为激光增益材料的可行性。
实施例2
一种碲酸盐玻璃,原料组成如表1中2-8#所示;
按照表1中2-8#玻璃组成的质量百分比,计算出相应的各组成的重量,并称取各原料组分;将原料研磨均匀形成混合料后,放入铂金坩埚中,并置于750~800℃的硅碳棒电炉中熔制20分钟得到熔融的玻璃液,在玻璃熔制过程中始终通入高纯氧气进行气氛保护以除去玻璃液中的水分。除去水分的玻璃液经均化澄清,然后快速浇注到已预热至300~350℃的模具上,后再放入已升温至所述玻璃液的250~300℃的马弗炉中,保温3小时后,然后关闭马弗炉,降温至室温,完全冷却后取出玻璃样品。
对玻璃的测试结果如下:
②将退火后的玻璃加工成10×20×1毫米的玻璃片并抛光。
②在980和650nm波长的激光二极管泵浦下测试其荧光光谱,分别如图1和2所示。实验表明,玻璃透明,无析晶。在980和650nm波长的激光二极管泵浦下均可以获得明显的中红外2.8μm荧光,当ZnCl2得含量增加时,荧光强度递增。适用于中红外2.8μm激光玻璃与光纤材料的制备及应用。
Claims (3)
2.如权利要求1所述的掺铒碲铋酸盐中红外玻璃的制备方法,其特征在于,该方法包括下列步骤:
(1)原料预备:按照玻璃组成的摩尔百分比,计算出相应各组成的重量,称取原料;
(2)制备技术:所有原料组分研磨均匀形成混合料后,放入铂金坩埚中,并置于750~800℃的硅碳棒电炉中熔制20~30分钟,均化和澄清后得到均匀无气泡的玻璃液;
(3)浇注:将步骤(2)得到的玻璃液浇注到已预热至300~350℃的模具上;
(4)退火:后再放入已升温至250~300℃的马弗炉中,保温2~3小时后,然后关闭马弗炉,降温至室温。
3.根据权利要求2所述的掺铒碲铋酸盐中红外玻璃的制备方法,其特征在于,在步骤(2)的熔制过程中以搅拌的形式使铂金坩埚中混合均匀排除气泡。
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