CN106396413B - 铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷及其制备方法 - Google Patents
铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷及其制备方法 Download PDFInfo
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Abstract
本发明涉及铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷及其制备方法,其物质的量百分组成为:4.5BaCO3‑3.5WO3‑35SiO2‑31B2O3‑25NaF‑0.2Sb2O3‑0.1Er2O3‑0.7Yb2O3。制备方法采用熔融晶化技术。发明的铒镱共掺上转换发光玻璃陶瓷的主晶相为钨酸钡,厚度为2mm的铒镱共掺上转换发光玻璃陶瓷在可见光区的透过率为85%,在980nm波长激发下,可见4个发射峰分别为484nm,530nm,549nm和653nm,其中484nm处的发射峰对应于Er3+的4F7/2→4I15/2跃迁,530nm和549nm处的绿光发射峰分别对应于Er3+的2H11/2,5S3/2→4I15/2跃迁,653nm处的红光发射峰对应于Er3+的4F9/2→4I15/2跃迁。而且,绿光与红光发射均为双光子过程。
Description
技术领域
本发明涉及玻璃陶瓷制备技术领域,具体地说涉及钨酸钡为晶相铒镱共掺上转换发光玻璃陶瓷及其制备方法。
背景技术
上转换发光材料以其独特的优势和广泛地应用价值备受关注。在众多稀土离子中,由于Er3+掺入到放大器中可以降低通信系统中的光损失成为现如今的研究热点。Yb3+作为敏化中心能非常有效的将在980nm激发下产生的能量传递给Er3+从而提高Er3+的发光强度,因此Er3+/Yb3+共掺的光学材料被广泛的研究。最近几年,M.Secu等人通过溶胶凝胶法制备了Er3+/Yb3+共掺的含LiYF4纳米晶的玻璃陶瓷并得到在该样品中红光与绿光发射均为双光子过程。V.K.Tikhomirov等人制备了Er3+/Yb3+共掺透明玻璃陶瓷并找到Yb3+和Er3+的最佳浓度比而且研究了激发态离子的衰变动力学。
钨酸盐的结构多属于白钨矿,稀土离子和碱金属无序地占据结构中二价阳离子的位置,且[WO4]2-本身就是较好的发光基质。四面体结构单元参与玻璃三维网络的构建,增强玻璃网络结构的紧密性,增大玻璃粘度,从而提高玻璃的析晶稳定性。近年来,C.Bouzidi等人通过固态熔融法制备了Eu3+/Sm3+共掺的BaWO4粉体并发现了Sm3+作为敏化剂可以在很大程度上加强Eu3+的发光强度。对于铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷还未见相关报道。
发明内容
本发明的目的在于提供一种铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷及其制备方法。
本发明是通过以下的技术方案来实现的:
一种铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷,其组分及其含量(物质的量百分比)如下:4.5BaCO3-3.5WO3-35SiO2-31B2O3-25NaF-0.2Sb2O3-0.1Er2O3-0.7Yb2O3。
本发明的铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷的制备方法,包括以下步骤:
1)按组分及含量计算称取各物质,并充分混合均匀,置于铂金坩埚中,放入硅钼炉中,升温至1450℃,使原料熔融成液态,并恒温1-2小时后,将坩埚中的液体倒在已预热的不锈钢模具上固化成型,迅速放入450℃马弗炉中,保温1小时,随炉降至室温,制得铒镱共掺透明玻璃;
2)将铒镱共掺透明玻璃放入箱式电阻炉中,采用一步析晶法,以5℃/分钟的升温速率升温至620℃,保温2小时,得到铒镱共掺玻璃陶瓷;
3)将制得的铒镱共掺玻璃陶瓷切割,然后用磨抛机对玻璃陶瓷进行双面研磨和抛光,最终得到铒镱玻璃陶瓷厚度为2mm。
采用X射线衍射分析确定铒镱共掺玻璃陶瓷的主晶相;采用紫外-可见-近红外分光光度计测量厚度为2mm的铒镱共掺玻璃陶瓷的光透过率;采用荧光光谱仪测量铒镱共掺玻璃陶瓷的上转换发光光谱。
铒镱共掺玻璃陶瓷的主晶相为钨酸钡。厚度为2mm铒镱共掺玻璃陶瓷在可见光区的透过率为85%。
附图说明
图1为铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷的X射线衍射分析谱图,该图兼作摘要附图。
图2为铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷的透过率曲线。
图3为铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷的上转换发射光谱图。
图4为铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷的上转换发光强度与激光器的激发功率之间的双常用对数图。
具体实施方式
下面结合实施例和附图对本发明作进一步说明,但不限于这些实施例。
称取各组分4.5BaCO3-3.5WO3-35SiO2-31B2O3-25NaF-0.2Sb2O3-0.1Er2O3-0.7Yb2O3(物质的量百分比),按照上述配比,称取原料共30克,并充分混合均匀,置于铂金坩埚中,放入硅钼炉中,升温至1450℃,使原料熔融成液态,恒温1小时后,将坩埚中的液体倒在已预热的不锈钢模具上固化成型,迅速放入450℃马弗炉中,保温1小时,随炉降至室温,制得铒镱共掺透明玻璃;将铒镱共掺透明玻璃样品放入箱式电阻炉中,以5℃/分钟的升温速率升温至620℃,保温2小时,随炉降至室温,得到铒镱共掺透明玻璃陶瓷;将制得的铒镱共掺透明玻璃陶瓷用切割机切割,然后进行研磨和抛光,最终得到铒镱共掺透明玻璃陶瓷样品厚度为2mm。采用X射线衍射分析确定铒镱共掺透明玻璃陶瓷的主晶相为钨酸钡,见附图1;采用紫外-可见-近红外分光光度计测量厚度为2mm的铒镱共掺透明玻璃陶瓷的光透过率,可见光区可达85%,见附图2;采用荧光光谱仪测量铒镱共掺透明玻璃陶瓷的上转换发光光谱,在980nm半导体激光器激发下,铒镱共掺透明玻璃陶瓷的上转换发射光谱见附图3,图中可见4个发射峰,分别位于波长为484nm,530nm,549nm和653nm,其中484nm处的发射峰为青色对应于Er3+的4F7/2→4I15/2跃迁,530nm和549nm处的发射峰为绿色分别对应于Er3+的2H11/2、5S3/2→4I15/2跃迁,653nm处的发射峰为红色对应于Er3+的4F9/2→4I15/2跃迁。改变半导体激光器的激发功率,测定不同激发功率下铒镱共掺透明玻璃陶瓷样品在484nm、530nm、549nm和653nm处的发光强度,然后对发光强度以及激发功率取双常用对数进行拟合,得到上转换发光强度与激光器的激发功率之间的双常用对数图见附图4所示。由图4可知484nm、530nm、549nm、653nm波长处的斜率分别为1.84、1.64、1.67、1.81,均接近2,这表明绿光与红光发射均为双光子过程。
当然,本发明还有很多实施例,在不背离本发明精神及实质的情况下,熟悉本领域的技术人员当可根据本发明做出相应的改变和变形,但这些相应的改变和变形都应属于本发明所附的权利要求保护范围内。
Claims (1)
1.一种铒镱共掺含钨酸钡晶相上转换发光玻璃陶瓷,其特征在于:该玻璃陶瓷的化学组成及其物质的量百分含量如下:4.5BaCO3-3.5WO3-35SiO2-31B2O3-25NaF-0.2Sb2O3-0.1Er2O3-0.7Yb2O3,该玻璃陶瓷的主晶相为钨酸钡,厚度为2mm的透明玻璃陶瓷在可见光区的透过率为85%,该玻璃陶瓷的制备方法由以下工艺步骤所组成:
1)按组分及含量计算称取各物质,并充分混合均匀,置于铂金坩埚中,放入硅钼炉中,升温至1450℃,使原料熔融成液态,并恒温1-2小时后,将坩埚中的液体倒在已预热的不锈钢模具上固化成型,迅速放入450℃马弗炉中,保温1小时,随炉降至室温,制得铒镱共掺透明玻璃;
2)将铒镱共掺透明玻璃放入箱式电阻炉中,采用一步析晶法,以5℃/分钟的升温速率升温至620℃,保温2小时,得到铒镱共掺玻璃陶瓷;
3)将制得的铒镱共掺玻璃陶瓷切割,然后用磨抛机对玻璃陶瓷进行双面研磨和抛光,最终得到铒镱共掺玻璃陶瓷厚度为2mm。
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