CN104445341B - 一种纯yag相的钇铝石榴石纳米粉体的制备方法 - Google Patents

一种纯yag相的钇铝石榴石纳米粉体的制备方法 Download PDF

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CN104445341B
CN104445341B CN201410678115.6A CN201410678115A CN104445341B CN 104445341 B CN104445341 B CN 104445341B CN 201410678115 A CN201410678115 A CN 201410678115A CN 104445341 B CN104445341 B CN 104445341B
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吴起白
张海燕
冯寅
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Guangdong University of Technology
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Abstract

本发明公开了一种纯YAG相的钇铝石榴石纳米粉体的制备方法，该方法通过略微增加反应溶液中铝离子的浓度，采用化学共沉淀法制备粉体，方法步骤依次为：配制硝酸铝和硝酸钇混合溶液；将上述混合溶液缓慢滴加到碳酸氢铵溶液中；搅拌、陈化及抽滤；干燥、研磨及煅烧；获得纯YAG相的钇铝石榴石纳米粉体，不含有其他中间相；所得粉体分散性较好，形状为棒状，平均颗粒尺寸约为150nm；本发明所得的粉体用于制备YAG透明激光陶瓷，还用于制备YAG荧光粉。

Description

一种纯YAG相的钇铝石榴石纳米粉体的制备方法
技术领域
本发明涉及一种纯YAG相的钇铝石榴石纳米粉体的制备方法。
背景技术
固体激光器在先进制造业、信息、能源、国防、医疗等领域均具有重大的应用价值，钇铝石榴石（YAG）单晶是目前运用最广泛，性能最优良的固体激光器工作基质，但具有生长周期较长，掺杂浓度较低，晶体尺寸小的局限。自从1995年日本科学家A.Ikesue成功制备出第一块有激光输出的Nd:YAG透明陶瓷，透明陶瓷研究受到了广泛重视。与单晶材料相比，透明激光陶瓷可实现大尺寸，大比例的掺杂，成本也相对较低。对制备低光学损耗的透明陶瓷而言，性能优良的纳米粉体是前提和基础。目前，制备YAG纳米粉体的方法主要有固相法、化学共沉淀法、均相沉淀法、溶胶-凝胶法等，其中化学共沉淀法是一种操作简单、成本低廉的粉体制备方法。
化学共沉淀法通常以硝酸铝和硝酸钇为原料，按摩尔比n(Y)：n(Al)=3:5称取一定质量的硝酸铝和硝酸钇配制成混合溶液，作为反应溶液；碳酸氢铵为沉淀剂，利用化学沉淀反应制备YAG纳米粉体。但由于在多组分体系中溶度积，沉淀速率的差别，难以形成确定精确化学计量比和组分完全均一的前驱粉体，煅烧前驱体后常有YAP、YAM等中间相出现，而中间相会对后续的陶瓷烧结产生不利影响。本发明提出了一种采用化学共沉淀法制备纯YAG相的钇铝石榴石纳米粉体的方法，通过调整反应溶液中铝离子浓度使沉淀形成的前驱物经煅烧后能够形成不含杂相的纯立方相YAG纳米粉体。
发明内容
本发明的目的在于提供一种采用化学共沉淀法制备不含有其它杂相的纯YAG相的钇铝石榴石纳米粉体的方法，此方法的关键在于略微增加反应溶液中铝离子的浓度，避免因铝离子的流失而产生中间相。
实现本发明目的的具体技术步骤为：
本发明提供的一种纯YAG相的钇铝石榴石纳米粉体的制备方法，该方法通过略微增加反应溶液中铝离子的浓度，采用化学共沉淀法制备粉体，方法步骤依次为：
（1）配制硝酸铝和硝酸钇混合溶液；
（2）将上述混合溶液缓慢滴加到碳酸氢铵溶液中；
（3）搅拌、陈化及抽滤；
（4）干燥、研磨及煅烧；获得纯YAG相的钇铝石榴石纳米粉体。
所述步骤（1）中，以纯度为99.99%的Al(NO3)3·9H2O和纯度为99.99%的Y(NO3)3·6H2O为原料，以离子水和无水乙醇为溶剂，去离子水与无水乙醇的体积比为2:1， 配制硝酸铝和硝酸钇混合溶液，其中Y3+：Al3+摩尔比为9:16。
所述步骤（2）中，利用去离子水配置1.2mol/L的碳酸氢铵溶液， 将步骤（1）中配制的硝酸铝和硝酸钇混合溶液以2mL/min的速率滴加到碳酸氢铵溶液中，同时搅拌溶液。
所述步骤（3）中，滴定完毕后继续搅拌1～2h，使共沉淀反应进行完全；然后将反应液放置陈化48h；再采用抽滤的方法，用去离子水和无水乙醇反复洗涤浆料各3次，得到滤饼。
所述步骤（4）中，将滤饼放在60～120℃干燥箱内干燥3～6h；把干燥后的样品研磨成粉末状，放入高温炉中1200℃煅烧3～5h，获得纯YAG相的钇铝石榴石纳米粉体。
本发明的得益效果是：
通过略微增加反应溶液中铝离子的浓度，即Y3+：Al3+摩尔比为9:16，而非常规的3:5， 沉淀反应形成的前驱体经过煅烧后可形成不含杂相的纯立方相YAG纳米粉体，过多或过少都会产生杂相。所得粉体分散性较好，形状为棒状，平均颗粒尺寸约为150nm。本发明所得的粉体可用于制备YAG透明激光陶瓷，还可以用于制备YAG荧光粉。
附图说明
图 1 本发明所制备的纯YAG相的钇铝石榴石纳米粉体的XRD图。在图1中，可见所得粉体的XRD结果为完全的YAG相，没有其他中间相存在。
图 2 本发明所制备的纯YAG相的钇铝石榴石纳米粉体的表面形貌图（SEM）。可见粉体颗粒平均尺寸约在150nm左右。
具体实施方式
1. 配制硝酸铝和硝酸钇混合溶液，其中Y3+：Al3+摩尔比为9:16；
以Al(NO3)3·9H2O(纯度为99.99%)和Y(NO3)3·6H2O(纯度为99.99%)为原料，以去离子水和无水乙醇（其体积比2:1）为溶剂， 配制Al(NO3)3·9H2O和Y(NO3)3·6H2O的混合溶液100mL，其中Y3+浓度为0.09mol/L，Al3+ 浓度为0.16mol/L，即Y3+：Al3+摩尔比为9:16。
2. 将混合溶液缓慢滴加到碳酸氢铵溶液中；
利用去离子水配制1.2mol/L的NH4HCO3溶液100mL， 将上述步骤1中配制的硝酸铝和硝酸钇混合溶液以2mL/min的速率滴加到碳酸氢铵溶液中，同时搅拌溶液。
3. 搅拌、陈化及抽滤
滴定完毕后继续搅拌1～2h，使共沉淀反应进行完全。然后将反应液放置陈化48h。再采用抽滤的方法，用去离子水和无水乙醇反复洗涤浆料各3次，得到滤饼。
4. 干燥、研磨及煅烧
将滤饼放在120℃干燥箱内干燥6h。把干燥后的样品研磨成粉末状，放入高温炉中1200℃煅烧3h，获得YAG粉体，XRD图（图1）证实为纯YAG相的钇铝石榴石纳米粉体。

Claims (3)

1.一种纯YAG相的钇铝石榴石纳米粉体的制备方法，其特征在于：采用化学共沉淀法制备粉体，其制备方法步骤如下：
(1)配制硝酸铝和硝酸钇混合溶液，以纯度为99.99％的Al(NO3)3·9H2O和纯度为99.99％的Y(NO3)3·6H2O为原料，以离子水和无水乙醇为溶剂，去离子水与无水乙醇的体积比为2:1，配制硝酸铝和硝酸钇混合溶液，其中Y3+：Al3+摩尔比为9:16；
(2)将上述混合溶液缓慢滴加到碳酸氢铵溶液中，利用去离子水配置1.2mol/L的碳酸氢铵溶液，将步骤(1)中配制的硝酸铝和硝酸钇混合溶液以2mL/min的速率滴加到碳酸氢铵溶液中，同时搅拌溶液；
(3)搅拌、陈化及抽滤；
(4)干燥、研磨及煅烧；获得纯YAG相的钇铝石榴石纳米粉体。
2.如权利要求1中所述的制备方法，其特征在于：所述步骤(3)中，滴定完毕后继续搅拌1～2h，使共沉淀反应进行完全；然后将反应液放置陈化48h；再采用抽滤的方法，用去离子水和无水乙醇反复洗涤浆料各3次，得到滤饼。
3.如权利要求1中所述的制备方法，其特征在于：所述步骤(4)中，将滤饼放在60～120℃干燥箱内干燥3～6h；把干燥后的样品研磨成粉末状，放入高温炉中1200℃煅烧3～5h，获得纯YAG相的钇铝石榴石纳米粉体。
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CN113264777B (zh) * 2021-04-26 2022-09-27 天津大学 一种具有高温抗热震性的氮化铝-铝酸钇复相陶瓷及制备方法

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