CN102303891A - 掺钕钆钪铝石榴石纳米粉体的制备方法 - Google Patents
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Abstract
本发明涉及掺钕钆钪铝石榴石（Nd:GSAG）纳米粉体的制备方法。掺钕钆钪铝石榴石纳米粉体的制备方法，其特征在于如下步骤实现：配制Gd(NO3)3、Nd(NO3)3、Sc(NO3)3、Al(NO3)3的摩尔浓度分别为：0.12－0.12xmol/L、0.12xmol/L、0.08mol/L、0.12mol/L，其中x=0.01,0.015,0.02。称取柠檬酸加入上述混合硝酸盐溶液，使混合溶液中柠檬酸的摩尔浓度为0.48mol/L；控制混合液温度为70-80℃，调节pH为7-8时，得到浅黄色溶液；加热浓缩，形成凝胶；继续加热，凝胶开始燃烧，待凝胶燃烧完全后，在容器底部得到前驱物粉体；收集前驱物粉体，研磨后放入马弗炉进行煅烧，在900℃恒温3h后随炉冷却，获得目标粉体。将溶胶凝胶方法与燃烧法相结合，制备设备简易，合成过程时间减少，能制备分散性好，纳米级别的粉体原料。
Description
技术领域
本发明涉及掺钕钆钪铝石榴石（Nd:GSAG）纳米粉体的制备方法，是一种采用sol-gel与燃烧法相结合的湿化学合成方法，属纳米材料制备技术领域。
背景技术
在空间探测领域，虽然水蒸气在温室效应、大气对流、云雾雨雪等重要气象过程中起了关键作用，但是由于其在大气中的含量虽然很少，获取整个大气对流层的高精度、高垂直分辨率的水蒸气廓线非常困难，到目前仍不能准确模拟水循环，这被认为是大气科学中的主要挑战。随着激光技术和弱信号探测技术的发展, 激光雷达在大气探测中扮演着日益重要的角色。其中差分吸收激光雷达技术（DIAL）单元组态可以测量任意方向的气体浓度，具有测量范围广（达到几千米），空间分辨率高的优点，大大提高了大气中微量气体的探测精度和灵敏度，使得准确测量大气水蒸气组分成为可能。综合考虑测量的需要和技术上的可行性，水蒸气940nm附近的936nm、942nm和944nm三个波段的吸收谱线可用于高精度的差分激光雷达吸收测量。过去20多年中，主要依赖OPO激光技术、拉曼频移激光技术或Ti宝石激光技术来获得这些波段的激光。采用这些技术的设备系统不仅复杂、昂贵，而且体积庞大，效率较低，已经不能满足现代空间激光雷达如WALES对效率、体积、寿命等的要求。激光二极管泵浦固体激光器（DPSSL）具有高效、紧凑、可靠、寿命长的优点，用于空间激光雷达有明显的优势，因此新型激光材料成为基本的物质条件。国内外最新的研究表明，Nd:GSAG晶体
激光器可获得了936、942nm附近波长激光，有望用作探测大气水蒸气的运行于935nm，942nm或944nm中任一波长的差分吸收雷达激光光源。国内外的激光透明陶瓷及激光器的研究表明：激光透明陶瓷具有不亚于单晶的激光性能及制备技术上的独特优势，在高功率、高效率激光器方面展现出具有巨大的应用潜力。因此，Nd:GSAG透明陶瓷的制备具有重要的意义。目前尚未见关于Nd:GSAG陶瓷制备的相关工作。对于制备高光学质量的Nd:GSAG透明陶瓷而言，分散性，烧结性能良好的纳米粉体原料是理想的选择。我们的实验借鉴湿化学方法，制备Nd:GSAG纳米粉体原料。
发明内容
发明目的
本发明的目的是针对溶胶－凝胶方法用时较长，效率不高的缺点，特提出改进的制备纳米粉体的湿化学方法。
技术方案
掺钕钆钪铝石榴石纳米粉体的制备方法，其特征在于如下步骤实现：
A、配制Gd(NO3)3、 Nd(NO3)3、Sc(NO3)3、Al(NO3)3的摩尔浓度分别为：0.12－0.12xmol/L、 0.12x mol/L、0.08mol/L、0.12mol/L，其中x =0.01, 0.015, 0.02；
B. 称取柠檬酸加入上述混合硝酸盐溶液，使混合溶液中柠檬酸的摩尔浓度为0.48 mol/L；控制混合液温度为70-80℃，调节pH为7-8时，得到浅黄色溶液；
C.加热浓缩，形成凝胶；继续加热，凝胶开始燃烧，待凝胶燃烧完全后，在容器底部得到前驱物粉体；
D. 收集前驱物粉体，研磨后放入马弗炉进行煅烧，在900℃恒温3h后随炉冷却，获得目标粉体。
有益效果
① 将溶胶凝胶方法与燃烧法相结合，制备设备简易，合成过程时间减少，能制备分散性好，纳米级别的粉体原料。
② 制备过程没有原料的损耗，避免了合成粉体的组分偏差。
附图说明
图1为制备Nd:GSAG纳米粉体的工艺流程图；
图2为目标粉体的XRD图谱；
图3为目标粉体的TEM图谱；
图4为目标样品在808nm激发下的发射光谱。
具体实施方式
现结合实施例，将本发明进一步详细叙述如下：
其中实验所用试剂的纯度为：
氧化钕 99.5％
氧化钆 99.995％
九水硝酸铝 分析纯
水 二次蒸馏水
硝酸 分析纯
柠檬酸 分析纯
氨水 分析纯
实施例1：本发明实施例的具体工艺步骤如下：
1. 称取一定质量的氧化钆，氧化钕和氧化钪，分别用稀硝酸完全溶解并定容；称取一定质量的九水硝酸铝，用二次蒸馏水溶解；
2. 根据(Gd1-x Nd x )3Sc2Al3O12中Nd3+掺杂浓度，用移液管分别量取一定体积的硝酸钆，硝酸钕，硝酸钪及硝酸铝溶液，将这些硝酸盐溶液均匀混合为适量体积的溶液，溶液中Gd(NO3)3, Nd(NO3)3, Sc(NO3)3, Al(NO3)3的摩尔浓度分别为：（0.12－0.12x）mol/L, 0.12x mol/L, 0.08mol/L, 0.12mol/L(x =0.01, 0.015, 0.02)。
3. 称取一定质量的柠檬酸加入上述混合硝酸盐溶液并搅拌至完全溶解，使混合溶液中柠檬酸的摩尔浓度为0.48 mol/L。用酸度计测定溶液的pH值，此时溶液显酸性，用滴管逐滴加入氨水，并加热，控制混合液温度为70-80℃，实时检测溶液的pH值，当pH为7-8时，停止加氨水，得到浅黄色溶液；
4. 将浅黄色溶液盛入体积较大的耐热容器中，放在电炉上加热，电炉功率不超过500W。
5. 持续加热，浅黄色溶液不断浓缩，形成凝胶；继续加热，调小加热功率，凝胶开始燃烧，待凝胶燃烧完全后，在容器底部得到黑褐色Nｄ:GSAG前驱物粉体；
6. 收集黑褐色粉体，研磨后放入马弗炉进行煅烧。在900度恒温3h后随炉冷却，获得白色粉体，在玻璃研钵内手工研磨白色粉体，获得目标粉体。
采用X射线粉末衍射技术（XRD），透射电镜（TEM）及光致发光光谱对该样品的晶相，形貌及发光性能进行了表征。见图2为目标粉体的XRD图谱。 衍射峰与GSAG (JCPDS 43-0659)一致，并且没有检测到杂峰，说明样品为Nd:GSAG多晶粉体。取5个衍射峰，用谢乐公式估算样品的平均晶粒尺寸，约为20nm。图3为目标粉体的TEM图谱，粉体分散性好，粒度均匀，颗粒尺寸分约为30-80nm。图4为目标样品在808nm激发下的发射光谱，粉体发光性能良好。
以上结果说明采用sol-gel与燃烧法相结合的技术，可以合成Nd:GSAG前驱物，将前驱物在900℃煅烧3h，可成功获得不同Nd3+掺杂的、分散性、发光性能良好的Nd:GSAG纳米粉体。
Claims (1)
1.掺钕钆钪铝石榴石纳米粉体的制备方法，其特征在于如下步骤实现：
A、配制Gd(NO3)3、 Nd(NO3)3、Sc(NO3)3、Al(NO3)3的摩尔浓度分别为：0.12－0.12xmol/L、 0.12x mol/L、0.08mol/L、0.12mol/L，其中x =0.01, 0.015, 0.02；
B. 称取柠檬酸加入上述混合硝酸盐溶液，使混合溶液中柠檬酸的摩尔浓度为0.48 mol/L；控制混合液温度为70-80℃，调节pH为7-8时，得到浅黄色溶液；
C.加热浓缩，形成凝胶；继续加热，凝胶开始燃烧，待凝胶燃烧完全后，在容器底部得到前驱物粉体；
D. 收集前驱物粉体，研磨后放入马弗炉进行煅烧，在900℃恒温3h后随炉冷却，获得目标粉体。
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| CN114014646A (zh) * | 2021-12-09 | 2022-02-08 | 营口理工学院 | 一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法 |
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Cited By (3)
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| CN111484848A (zh) * | 2020-04-27 | 2020-08-04 | 中国科学院长春应用化学研究所 | 一种近红外发光材料及其制备方法 |
| CN111484848B (zh) * | 2020-04-27 | 2021-06-15 | 中国科学院长春应用化学研究所 | 一种近红外发光材料及其制备方法 |
| CN114014646A (zh) * | 2021-12-09 | 2022-02-08 | 营口理工学院 | 一种柠檬酸螯合法制备纳米铝酸钆粉体材料的方法 |
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| CN102303891B (zh) | 2013-02-27 |
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