CN101270128B - 8-羟基喹啉铝纳米晶的制备方法 - Google Patents
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Abstract
本发明提供一种8-羟基喹啉铝纳米晶的制备方法，其包括以下步骤：将8-羟基喹啉铝粉末溶解于有机溶剂中，得到溶液A；将表面活性剂溶解于水中，得到溶液B；将溶液A与溶液B通过剧烈搅拌或强力超声均匀混合后，得到均一的乳液C；在40℃至90℃的温度下，将乳液C搅拌蒸发或减压蒸馏2至8小时以去除有机溶剂，离心分离后即得到8-羟基喹啉铝纳米晶。该制备方法操作简单、能耗低、适于工业化生产，且该方法制备所得的8-羟基喹啉铝纳米晶易于通过简单的旋涂法形成均一、致密的膜。
Description
技术领域
本发明涉及一种8-羟基喹啉铝的制备方法，尤其涉及8-羟基喹啉铝纳米晶的制备方法。
背景技术
8-羟基喹啉铝(Alq3)具有很高的热稳定性、良好的化学稳定性、优异的电子传输性能和发光性能，被广泛地应用于有机发光二极管、大屏幕显示器、场发射薄膜、荧光标记等。随着当今纳米科学与技术的不断推广，Alq3纳米晶的制备已成为人们关注的热点。
现有的Alq3纳米晶的制备主要是气相法，如：Pemg Tsong-Pyng等人采用蒸汽浓缩的方法制备Alq3纳米球和纳米线，但是未得到结晶的纳米球；YaoJiannian等人采用吸附辅助物理气相沉积的方法制备Alq3纳米线。上述制备Alq3纳米晶的方法操作复杂，需要特殊的仪器设备，还需要较高的的反应温度及消耗大量的保护气体，有些甚至是价格昂贵的稀有气体，这些都大大增加了Alq3纳米晶的制备成本，所以不利于大规模生产。同时，上述方法制备的Alq3纳米晶难于通过简单的方法形成形貌均一、致密的膜，因些又限制了其实际应用。
有鉴于此，提供一种操作简单、低能耗、易于工业化且产物易于简单成膜的Alq3纳米晶是必要的。
发明内容
一种8-羟基喹啉铝纳米晶的制备方法，其包括以下步骤：将8-羟基喹啉铝粉末溶解于有机溶剂中，得到溶液A；将适量表面活性剂溶解于水中，得到溶液B，且所述表面活性剂为十六烷基三甲基溴化铵或十二烷基硫酸钠；将溶液A与溶液B通过剧烈搅拌或强力超声均匀混合后，得到均一的乳液C；在40℃至90℃的温度下，将乳液C搅拌蒸发或减压蒸馏2至8小时；离心分离后即得到8-羟基喹啉铝纳米晶。
所述A溶液中8-羟基喹啉铝的浓度范围为6.0毫克/毫升至10.0毫克/毫升之间。
所述B溶液中表面活性剂的浓度范围为1.5毫克/毫升至4.0毫克/毫升之间。
所述有机溶剂为丙酮、N，N-二甲基甲酰胺、三氯甲烷、二氯甲烷及二甲亚砜中至少一种。
本发明采用液相法合成8-羟基喹啉铝纳米晶，与现有技术相比，该制备方法具有如下优点：操作简单、无需特殊的仪器设备、实验条件温和，因而可节约大量的能源；该制备过程中蒸发出的有机溶剂经冷却、收集并稍作分离后便可重复利用，因而可节约大量的原材料；该方法制备的Alq3纳米晶易于分散在水中以形成Alq3的胶体，而后通过旋涂的方法即可形成均一、致密的膜，从而避免了传统真空蒸镀法形成Alq3膜的高温及耗能问题。
附图说明
图1是本发明第一实施例制备的8-羟基喹啉铝纳米棒的扫描电镜(SEM)照片。
图2是本发明第一实施例制备的8-羟基喹啉铝纳米棒的透射电镜(TEM)照片。
图3是本发明第一实施例制备的8-羟基喹啉铝纳米棒的多晶X射线衍射(XRD)图。
图4是本发明第二实施例制备的8-羟基喹啉铝纳米棒的SEM照片。
图5是本发明第三实施例制备的8-羟基喹啉铝纳米球的SEM照片。
图6是图5的放大图。
图7是本发明第三实施例制备的8-羟基喹啉铝纳米球的质谱图。
具体实施方式
本发明提供一种Alq3纳米晶的制备方法，其具体步骤包括：(1)将8-羟基喹啉铝粉末溶解于有机溶剂中，得到8-羟基喹啉铝的浓度范围为6.0毫克/毫升至10.0毫克/毫升之间的溶液A；(2)将适量表面活性剂溶解于水中，得到表面活性剂的浓度范围为1.5毫克/毫升至4.0毫克/毫升之间的溶液B，；(3)将溶液A与溶液B通过剧烈搅拌或强力超声均匀混合后，得到均一的乳液C；(4)在40℃至90℃的温度下，将乳液C搅拌蒸发或减压蒸馏2至8小时以充分去除有机溶剂，离心分离后即得到8-羟基喹啉铝纳米晶。最后，将8-羟基喹啉铝纳米晶分散于水中，以避免其再次团聚。
表面活性剂为聚乙烯基吡咯烷酮(PVP)、十六烷基三甲基溴化铵(CTAB)、十二烷基硫酸钠(SDS)及十二烷基苯磺酸钠(SDBS)中至少一种。有机溶剂为丙酮、N，N-二甲基甲酰胺、三氯甲烷、二氯甲烷及二甲亚砜中至少一种。制备过程中蒸发出的有机溶剂经冷却、收集并稍作分离后便可重复利用。
制得的Alq3纳米晶可为直径为300纳米至1000纳米、长度为1至10微米的纳米棒或者直径为50纳米至300纳米的纳米球。Alq3纳米晶的形貌可通过控制表面活性剂的种类及添加量来控制，如：采用CTAB为表面活性剂，可制得Alq3纳米棒；采用SDS为表面活性剂，可制得Alq3纳米球；表面活性剂的添加量多，制得的Alq3纳米棒的长径比(长度/直径)大、Alq3纳米球的直径小；表面活性剂的添加量少，制得的Alq3纳米棒的长径比小、Alq3纳米球的直径大。该方法制备的Alq3纳米晶具有较好的分散性。
下面将结合附图对本发明实施例作进一步的详细说明。
实施例一：
将8毫克(mg)Alq3粉末溶解于1毫升(ml)氯仿(CHCl3)中，30mg CTAB溶解于16ml水中，将上述两溶液混合后以120瓦(w)功率超声并不断搅拌，得到均一的乳液，将所得乳液在60℃温度下搅拌蒸发约4小时以充分去除CHCl3，高速离心分离，即得到直径约为650纳米(nm)，长度约为5至10微米(μm)的Alq3纳米棒。最后，将所得Alq3纳米棒分散于水中，以避免其再次团聚。请参阅图1及图2分别为第一实施例制备的Alq3纳米棒的扫描电镜及透射电镜照片。请参阅图3为第一实施例制备的Alq3纳米棒的多晶X射线衍射(XRD)图，由图3可知Alq3纳米晶为α相晶体。
实施例二：
将20mgAlq3粉末溶解于2ml CHCl3中，50mg CTAB溶解于20ml水中，将上述两溶液混合后以120w功率超声并不断搅拌，得到均一的乳液，将所得乳液在60℃温度下搅拌蒸发约4小时以充分去除CHCl3及水，高速离心分离，即得到直径约为900nm，长度约为1.5至2μm的Alq3纳米棒。最后，将所得Alq3纳米棒分散于水中，以避免其再次团聚。请参阅图4为第二实施例制备的Alq3纳米棒的扫描电镜照片。
实施例三：
将8mgAlq3粉末溶解于1ml CHCl3中，60mg SDS溶解于16ml水中，将上述两溶液混合后以120w功率超声并不断搅拌，得到均一的乳液，将所得乳液在60℃温度下搅拌蒸发约4小时以充分去除CHCl3，高速离心分离，即得到直径约为100至270nm的Alq3纳米球。最后，将所得Alq3纳米球分散于水中，以避免其再次团聚。请参阅图5及图6为第三实施例制备的Alq3纳米球的扫描电镜照片。请参阅图7为第三实施例制备的Alq3纳米球的质谱图，由图7可知纳米球的成分为Alq3。
与现有技术相比较，该制备方法具有如下优点：操作简单、无需特殊的仪器设备、实验条件温和，因而可节约大量的能源；该制备过程中蒸发出的有机溶剂经冷却、收集并稍作分离后便可重复利用，因而可节约大量的原材料；该方法制备的Alq3纳米晶易于分散在水中以形成Alq3的胶体，而后通过旋涂的方法即可形成均一、致密的膜，从而避免了传统真空蒸镀法形成Alq3膜的高温及耗能问题。因此该方法可广泛地应用于大规模地工业化生产中。
另外，本领域技术人员还可在本发明精神内做其它变化。当然，这些依据本发明精神所做的变化，都应包含在本发明所要求保护的范围之内。
Claims (6)
1.一种8-羟基喹啉铝纳米晶的制备方法，其包括以下步骤：将8-羟基喹啉铝粉末溶解于有机溶剂中，得到溶液A；
将表面活性剂溶解于水中，得到溶液B，且所述表面活性剂为十六烷基三甲基溴化铵或十二烷基硫酸钠；
将溶液A与溶液B均匀混合后，得到均一的乳液C；
在40℃至90℃的温度下去除乳液C中的有机溶剂，离心分离后即得到8-羟基喹啉铝纳米晶。
2.如权利要求1所述的8-羟基喹啉铝纳米晶的制备方法，其特征在于，A溶液中8-羟基喹啉铝的浓度范围为6.0毫克/毫升至10.0毫克/毫升之间。
3.如权利要求1所述的8-羟基喹啉铝纳米晶的制备方法，其特征在于，B溶液中表面活性剂的浓度范围为1.5毫克/毫升至4.0毫克/毫升之间。
4.如权利要求1所述的8-羟基喹啉铝纳米晶的制备方法，其特征在于，有机溶剂为丙酮、N，N-二甲基甲酰胺、三氯甲烷、二氯甲烷及二甲亚砜中至少一种。
5.如权利要求1所述的8-羟基喹啉铝纳米晶的制备方法，其特征在于，均匀混合溶液A与溶液B的方法为剧烈搅拌或强力超声。
6.如权利要求1所述的8-羟基喹啉铝纳米晶的制备方法，其特征在于，去除乳液C中有机溶剂的方法为搅拌蒸发或减压蒸馏，时间为2至8小时。
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| Application Number | Priority Date | Filing Date | Title |
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| CN200710073648.1A CN101270128B (zh) | 2007-03-23 | 2007-03-23 | 8-羟基喹啉铝纳米晶的制备方法 |
| US12/002,142 US7880003B2 (en) | 2007-03-23 | 2007-12-14 | Method for making tris (8-hydroxyquinoline) nano-crystal |
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| CN104529892B (zh) * | 2015-01-28 | 2017-02-01 | 山东大学 | 一种自组装8‑羟基喹啉铝结晶微/纳米颗粒的制备方法 |
| CN104630897B (zh) * | 2015-01-28 | 2017-05-31 | 山东大学 | 一种8‑羟基喹啉金属配合物结晶微/纳米棒的制备方法 |
| CN105200524B (zh) * | 2015-09-11 | 2018-05-15 | 山东大学 | 一种8-羟基喹啉金属配合物微/纳米管及其制备方法 |
| CN105780125B (zh) * | 2016-01-18 | 2019-05-17 | 上海多磨新材料科技有限公司 | 介观尺度线条状有机晶体的制备方法 |
| KR102112842B1 (ko) * | 2018-02-09 | 2020-05-19 | (주) 파마젠 | 리튬 퀴놀레이트 및 리튬 퀴놀레이트 나노로드 결정의 제조방법 |
| CN111117605B (zh) * | 2019-12-26 | 2021-01-05 | 北京理工大学 | 一种有机铝纳米晶及其制备方法和应用 |
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