CN105506552B - 一种纳米Sn球的制备方法 - Google Patents

一种纳米Sn球的制备方法 Download PDF

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CN105506552B
CN105506552B CN201610028075.XA CN201610028075A CN105506552B CN 105506552 B CN105506552 B CN 105506552B CN 201610028075 A CN201610028075 A CN 201610028075A CN 105506552 B CN105506552 B CN 105506552B
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张麦丽
张方辉
牟强
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Shaanxi University of Science and Technology
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Abstract

本发明提供一种纳米Sn球的制备方法：1)在基板上涂覆一层松香；2)在涂覆的松香上制备一层Sn膜，得到样片；将样片放置在热处理设备内进行热处理，使Sn膜转变为离散分布在松香上的多个纳米Sn球；3)将热处理后的样片放入无水乙醇中，利用无水乙醇将松香溶化，使纳米Sn球与基板分离；4)经过步骤3)后，用无水乙醇清洗纳米Sn球。本发明制备得到的纳米Sn球发光性能较好，可以作为量子点进行应用；本发明采用固体作为原材料，纳米Sn球的直径大小取决于Sn膜的厚度，且所用试剂廉价、无毒，从而使本发明的制备方法具有操作简单、安全性高的优点。

Description

一种纳米Sn球的制备方法
技术领域
本发明属于显示领域，具体涉及一种量子点用的纳米Sn(锡)球的制备方法。
背景技术
量子点是由有限数目的原子组成，三个维度尺寸均在纳米数量级。量子点一般为球形或类球形，是由半导体材料制成的、稳定直径在2～20nm的纳米粒子。作为一种新颖的半导体纳米材料，量子点具有许多独特的纳米性质。
目前，量子点的制备主要有两种方式：有机相制备和水相制备。有机相制备具有荧光量子产率高、较窄的荧光半峰宽、较好的分散性和稳定性；但存在试剂毒性强、实验成本高、操作安全性低等诸多缺点。水相制备具有试剂无毒、廉价、操作简单等优点，但发光性能较差。
发明内容
本发明的目的在于提供一种纳米Sn球的制备方法。
为达到上述目的，本发明采用了以下技术方案：
1)在基板上涂覆一层松香；
2)在涂覆的松香上制备一层厚度≤10μm的Sn膜，得到样片；将样片放置在热处理设备内进行热处理，使Sn膜转变为离散分布在松香上的多个纳米Sn球；
3)将热处理后的样片放入无水乙醇中，利用无水乙醇将松香溶化，使纳米Sn球与基板分离；
4)经过步骤3)后，用无水乙醇清洗纳米Sn球。
所述基板的材料采用玻璃或塑料。
所述基板在涂覆松香前进行清洗，所述清洗的方法为超声清洗、刷洗或高压水流清洗。
所述松香的涂覆方法为印刷、旋涂或喷墨打印。
所述Sn膜的制备方法采用真空蒸镀或离子溅射。
所述热处理设备采用烘箱或马弗炉。
所述热处理的温度为200～400℃，热处理的时间为1～4h。
所述步骤4)具体包括以下步骤：用无水乙醇对步骤3)分离得到的纳米Sn球反复进行离心清洗，直到去除该纳米Sn球表面的松香。
本发明的有益效果体现在：
本发明所述纳米Sn球的制备方法制备得到的纳米Sn球发光性能较好，可以作为量子点进行应用；本发明采用固体作为原材料，纳米Sn球的直径大小取决于Sn膜的厚度，且所用试剂(如松香、无水乙醇)廉价、无毒，从而使本发明的制备方法具有操作简单、安全性高的优点。
附图说明
图1为本发明所述样片的示意图；
图2为本发明所述样片经过热处理后的示意图；
图中：1为基板，2为松香，3为Sn膜，4为Sn球。
具体实施方式
下面结合附图和实施例对本发明作详细说明。
1)基板清洗：
将1英寸的玻璃基板分别采用刷洗、在无水乙醇中超声清洗10min、用纯水超声清洗10min后，待用。刷洗主要是用来清洗基板表面的微粒，无水乙醇中超声清洗主要是为了清洗基板表面的有机物，纯水中超声清洗是为了清洗基板表面残留的乙醇；清洗有利于松香在玻璃表面的铺展，可以得到均匀平整的膜；
2)松香的涂覆：
将松香加热软化，然后采用印刷法在玻璃基板1表面上涂敷一层松香2，厚度为1μm；
3)Sn膜的制备：
待涂敷的松香2自然冷却至室温后，采用真空蒸镀的方法在松香2上制备一层Sn膜3，真空蒸镀的条件为：真空度为4×10-3Pa，蒸发时电流为100A，蒸发厚度为100nm，最终制备得到的样片结构如图1所示；
4)样片的热处理：
采用马弗炉对样片进行热处理，热处理温度为300℃、时间为2h；样片经热处理，使松香表面的Sn熔化，松香没有太大变化，Sn熔化后，由于与松香不浸润，依靠自身的表面张力形成Sn球4，如图2所示；
5)Sn球分离：
将热处理后的样片放入无水乙醇中(热处理后直接放入或者冷却一段时间后放入都可以)，利用无水乙醇将玻璃基板上的松香溶化，使Sn球与玻璃基板剥离，取出玻璃基板，即得到分散有Sn球的松香无水乙醇溶液；
6)Sn球清洗：
将分散有Sn球的松香无水乙醇溶液进行离心处理，使Sn球在试管底部形成团聚，然后去除上层液体；然后用无水乙醇对Sn球进行10次离心清洗(即用无水乙醇分散，然后离心，弃去上清，反复进行10次)，从而去除Sn球表面的松香(显微镜观察)。
将上述步骤6)得到的Sn球加入无水乙醇中，经超声分散，形成Sn球无水乙醇分散系；然后按以下步骤进行性能检测：
发光性能的检测：采用波长为450nm的蓝光照射本实施例所制备的所有Sn球，可以检测到绿光和红光。
粒径的检测：本实施例制备得到的Sn球的粒径为50～120nm，使用时可以根据需要进行筛选，直径较大的Sn球在450nm蓝光照射下可以得到红光，直接较小的Sn球在450nm蓝光照射下可以得到绿光。
其他实施例表明，增加Sn膜的厚度(例如，1μm左右)，则可以得到粒径更大的Sn球(在450nm蓝光照射下得到相应红光)，减小Sn膜的厚度，则可以得到粒径更小的Sn球(在450nm蓝光照射下可以得到相应绿光甚至蓝光)。

Claims (8)

1.一种Sn球的制备方法，其特征在于：包括以下步骤：
1)在基板上涂覆一层松香；
2)在涂覆的松香上制备一层厚度≤10μm的Sn膜，得到样片；将样片放置在热处理设备内进行热处理，使Sn膜转变为离散分布在松香上的多个Sn球；
3)将热处理后的样片放入无水乙醇中，利用无水乙醇将松香溶化，使Sn球与基板分离；
4)经过步骤3)后，用无水乙醇清洗Sn球。
2.根据权利要求1所述一种纳米Sn球的制备方法，其特征在于：所述基板的材料采用玻璃或塑料。
3.根据权利要求1所述一种Sn球的制备方法，其特征在于：所述基板在涂覆松香前进行清洗，所述清洗的方法为超声清洗、刷洗或高压水流清洗。
4.根据权利要求1所述一种Sn球的制备方法，其特征在于：所述松香的涂覆方法为印刷、旋涂或喷墨打印。
5.根据权利要求1所述一种Sn球的制备方法，其特征在于：所述Sn膜的制备方法采用真空蒸镀或离子溅射。
6.根据权利要求1所述一种Sn球的制备方法，其特征在于：所述热处理设备采用烘箱或马弗炉。
7.根据权利要求1所述一种Sn球的制备方法，其特征在于：所述热处理的温度为300～400℃，热处理的时间为1～4h。
8.根据权利要求1所述一种Sn球的制备方法，其特征在于：所述步骤4)具体包括以下步骤：用无水乙醇对步骤3)分离得到的Sn球反复进行离心清洗，直到去除该Sn球表面的松香。
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