CN106006731A - 一种稀土钒酸钇、制备方法及应用 - Google Patents
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Abstract
本发明公开了一种稀土钒酸钇、制备方法及应用，配置悬浮液，用去离子水和三亚乙基四胺溶液配置硝酸钇和正钒酸钠的悬浮液，所述悬浮液中，Y3+离子和VO4 3‑离子的摩尔浓度比为1.0～1.2：1，三亚乙基四胺TETA和H2O的体积比为1:1～17；水热反应制备米粒状钒酸钇，将上述悬浮液转移至密闭容器中，密封后在50～200℃反应8～24h，收集固体得到米粒状钒酸钇。本发明制得的产物纯度高，使用原料组分少，配比条件更易调控，制备工艺简单，成本低廉，能够制得均匀一致的米粒状钒酸钇。
Description
技术领域
本发明涉及一种用于制备稀土钒酸钇的方法，尤其涉及的是一种稀土钒酸钇、制备方法及应用。
背景技术
近年来，稀土钒酸盐(LnVO4)由于具有电子结构独特、原子磁矩大和自旋轨道效应强等效应，使其显现出磁性、光催化活性、化学和热稳定性、导电性、气敏性等良好的材料性能，因而在催化、发光材料、激光基质材料、磷光材料、介电材料、磁阻材料等领域得到了广泛的应用，尤其稀土钒酸盐发光材料在国内外的发展速度惊人，形成了相当大的生产规模和广阔的市场，其产值和经济效益都很高，从而为许多专家学者所关注。
目前，关于钒酸钇的制备方法有超声法、溶胶凝胶法、固相法等等。超声法反应不易控制、有副反应发生，微波反应器价格昂贵，只能限制在小规模合成上；溶胶凝胶法过程所需时间较长，溶胶中存在大量微孔，在干燥过程中又将会逸出许多气体及有机物，并产生收缩；固相法制得产品不易均匀，微粒易团聚，微粒直径分布宽。因此，急需研发一种操作简单、耗时短、绿色环保的钒酸钇制备方法。
发明内容
本发明的目的在于克服现有技术的不足，提供了一种稀土钒酸钇、制备方法及应用，实现快速的稀土钒酸钇的合成。
本发明是通过以下技术方案实现的，本发明包括以下步骤：
(1)配置悬浮液
使用去离子水和三亚乙基四胺溶液配置硝酸钇和正钒酸钠的悬浮液，所述悬浮液中，Y3+离子和VO4 3-离子的摩尔浓度比为1.0～1.2：1，三亚乙基四胺TETA和H2O的体积比为1:1～17；
(2)水热反应制备米粒状钒酸钇
将上述悬浮液转移至密闭容器中，密封后在50～200℃反应8～24h，收集固体得到米粒状钒酸钇。
所述步骤(1)中，所述悬浮液的配置包括以下步骤：
(11)首先将硝酸钇溶解于去离子水中，再加入三亚乙基四胺溶液配置得到硝酸钇溶液；
(12)然后将正钒酸钠溶解在去离子水中得到正钒酸钠溶液；
(13)在室温下将步骤(11)的硝酸钇溶液和步骤(12)的正钒酸钠溶液迅速混合搅拌即可。
作为本发明的优选方式之一，所述步骤(1)中，三亚乙基四胺TETA和H2O的体积比分别为1:1，1:3，1:8，1：17。
作为本发明的优选方式之一，所述步骤(2)中的密闭容器为带聚四氟乙烯内衬的不锈钢反应釜。
作为本发明的优选方式之一，所述悬浮液在密封容器中密封后，放置于烘箱中180℃反应12h。
一种如所述制备方法制得的稀土钒酸钇。
所述稀土钒酸钇为结构均匀一致的米粒结构。
一种稀土钒酸钇在制备发光材料中的应用。将本发明的稀土钒酸钇作为基质应用在发光材料中，通过掺杂，获得具有优良的发光效率和化学稳定性。
稀土钒酸盐材料有很丰富的光学特性，如光致发光，电致发光，荧光特性，吸光特性等。而YVO4:Ln(Ln＝Eu，Tm，Dy)是一种性能优良的红色荧光材料，其中稀土离子的4f电子跃迁所对应的发射为锐线光谱，受外场的影响小，并且具有优良的发光效率和化学稳定性，可广泛应用于高质量的彩色电视机荧光粉，灯用荧光粉，医用荧光粉，光学玻璃，激光材料等。由此可见，以纳米级稀土钒酸盐为基质的发光材料是一种很有应用前途的发光材料。
本发明相比现有技术具有以下优点：本发明制得的产物纯度高，使用原料组分少，配比条件更易调控，制备工艺简单，成本低廉，能够制得均匀一致的米粒状钒酸钇。
附图说明
图1为实施例1～4所得到的米粒状钒酸钇的X-射线衍射图；
图2为实施例1得到的米粒状钒酸钇场发射扫描电镜照片；
图3为实施例2得到的米粒状钒酸钇场发射扫描电镜照片；
图4为实施例3得到的米粒状钒酸钇场发射扫描电镜照片；
图5为实施例4得到的米粒状钒酸钇场发射扫描电镜照片。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1
本实施例以硝酸钇、三亚乙基四胺和正钒酸钠为原料，制备稀土钒酸钇包括以下具体步骤：
(1)配制悬浮液
称取1mmol用0.4022g硝酸钇Y(NO3)3﹒6H2O溶解于12ml去离子水中，再加入1ml三亚乙基四胺配成A液，再称取1mmol正钒酸钠Na3VO4溶解于5ml去离子水中，配成B液，在室温下将A液和B液迅速混合搅拌即可得混合悬浮液，其中Y3+/VO4 3-摩尔浓度比为1:1，TETA/H2O体积比为1:17；
(2)水热反应
将悬浮液转移至密闭容器中，密封后置于烘箱中150℃反应8h后，收集固体即为米粒状钒酸钇。
实施例2
本实施例以硝酸钇、三亚乙基四胺和正钒酸钠为原料，制备稀土钒酸钇的方法包括以下具体步骤：
(1)配制悬浮液
称取1mmol硝酸钇Y(NO3)3﹒6H2O溶解于11ml去离子水中，再加入2ml三亚乙基四胺配成A液，再称取1mmol正钒酸钠Na3VO4溶解于5ml去离子水中，配成B液，在室温下将A液和B液迅速混合搅拌即可得混合悬浮液，其中Y3+/VO4 3-摩尔浓度比为1:1，TETA/H2O体积比为1:8；
(2)水热反应
将悬浮液转移至密闭容器中，密封后置于烘箱中200℃反应24h后，收集固体即为米粒状钒酸钇。
实施例3
本实施例以硝酸钇、三亚乙基四胺和正钒酸钠为原料，制备稀土钒酸钇的方法包括以下具体步骤：
(1)配制悬浮液
称取1mmol硝酸钇Y(NO3)3﹒6H2O溶解于8.5ml去离子水中，再加入4.5ml三亚乙基四胺配成A液，再称取1mmol正钒酸钠Na3VO4溶解于5ml去离子水中，配成B液，在室温下将A液和B液迅速混合搅拌即可得混合悬浮液，其中Y3+/VO4 3-摩尔浓度比为1:1，TETA/H2O体积比为1:3；
(2)水热反应
将悬浮液转移至密闭容器中，密封后置于烘箱中170℃反应20h后，收集固体即为米粒状钒酸钇。
实施例4
本实施例以硝酸钇、三亚乙基四胺和正钒酸钠为原料，制备稀土钒酸钇的方法包括以下具体步骤：
(1)配制悬浮液
称取1mmol硝酸钇Y(NO3)3﹒6H2O溶解于4ml去离子水中，再加入9ml三亚乙基四胺配成A液，再称取1mmol正钒酸钠Na3VO4溶解于5ml去离子水中，配成B液，在室温下将A液和B液迅速混合搅拌即可得混合悬浮液，其中Y3+/VO4 3-摩尔浓度比为1:1，TETA/H2O体积比为1:1；
(2)水热反应
将悬浮液转移至密闭容器中，密封后置于烘箱中200℃反应8h后，收集固体即为米粒状钒酸钇。
将实施例1的产物用去离子水和无水乙醇洗涤，80℃下烘干6h，进行测试表征。图1为所得产物的XRD图谱，由图上可以看出，证明所得产物为YVO4；图2为实施例1产物的场发射扫描电镜照片，显示产物为米粒状结构。
将实施例2的产物用去离子水和无水乙醇洗涤，80℃下烘干6h，进行测试表征。图1为所得产物的XRD图谱，证明所得产物为YVO4；图3为实施例2产物的场发射扫描电镜照片，显示产物为米粒状结构。
将实施例3的产物用去离子水和无水乙醇洗涤，80℃下烘干6h，进行测试表征。图1为所得产物的XRD图谱，证明所得产物为YVO4；图4为实施例2产物的场发射扫描电镜照片，显示产物为米粒状结构。
将实施例4的产物用去离子水和无水乙醇洗涤，80℃下烘干6h，进行测试表征。图1为所得产物的XRD图谱，证明所得产物为YVO4；图5为实施例2产物的场发射扫描电镜照片，显示产物为米粒状结构。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种稀土钒酸钇的制备方法，其特征在于，包括以下步骤：
(1)配置悬浮液
使用去离子水和三亚乙基四胺溶液配置硝酸钇和正钒酸钠的悬浮液，所述悬浮液中，Y3+离子和VO4 3-离子的摩尔浓度比为1.0～1.2：1，三亚乙基四胺TETA和H2O的体积比为1:1～17；
(2)水热反应制备米粒状钒酸钇
将上述悬浮液转移至密闭容器中，密封后在50～200℃反应8～24h，收集固体得到米粒状钒酸钇。
2.根据权利要求1所述的一种稀土钒酸钇的制备方法，其特征在于，所述步骤(1)中，所述悬浮液的配置包括以下步骤：
(11)首先将硝酸钇溶解于去离子水中，再加入三亚乙基四胺溶液配置得到硝酸钇溶液；
(12)然后将正钒酸钠溶解在去离子水中得到正钒酸钠溶液；
(13)在室温下将步骤(11)的硝酸钇溶液和步骤(12)的正钒酸钠溶液迅速混合搅拌即可。
3.根据权利要求1所述的一种稀土钒酸钇的制备方法，其特征在于，所述步骤(1)中，三亚乙基四胺TETA和H2O的体积比分别为1:1，1:3，1:8，1：17。
4.根据权利要求1所述的一种稀土钒酸钇的制备方法，其特征在于，所述步骤(2)中的密闭容器为带聚四氟乙烯内衬的不锈钢反应釜。
5.根据权利要求1所述的一种稀土钒酸钇的制备方法，其特征在于，所述悬浮液在密封容器中密封后，放置于烘箱中180℃反应12h。
6.一种如权利要求1～5任一项所述制备方法制得的稀土钒酸钇。
7.根据权利要求6所述的一种稀土钒酸钇，其特征在于，所述稀土钒酸钇为结构均匀一致的米粒结构。
8.根据权利要求6所述的一种稀土钒酸钇，其特征在于，所述稀土钒酸钇的长度为150～550nm，粒径为10～100nm。
9.一种如权利要求6所述的稀土钒酸钇在制备发光材料中的应用。
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| CN101624206A (zh) * | 2009-08-07 | 2010-01-13 | 南开大学 | 稀土金属氢氧化物或钒酸盐纳米材料的制备方法及应用 |
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