CN116814262A - 一种基于铋基钙钛矿量子点荧光传感器的制备方法及其应用 - Google Patents
一种基于铋基钙钛矿量子点荧光传感器的制备方法及其应用 Download PDFInfo
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Abstract
本发明涉及一种基于铋基钙钛矿量子点荧光传感器的制备方法，本通过配体辅助再沉淀法制备了铋基钙钛矿量子点，并用于Cr(Ⅵ)的检测：首先将氯化铯、氯化铋、壳聚糖溶于1‑烯丙基‑3‑甲基‑氯化咪唑([AMIM]Cl)和二甲基亚砜的混合溶液中，用做前驱体；然后取适量前驱体滴入混合油酸的乙醇溶剂中，加热搅拌，离心过滤得上层清液，即为[AMIM]Cl/CS‑Cs3Bi2Cl9量子点荧光传感器，并将其应用于水中Cr(Ⅵ)的检测。本发明制备的[AMIM]Cl/CS‑Cs3Bi2Cl9量子点在370nm的激发波长下，于440nm处具有明亮蓝色发光。
Description
技术领域
本发明涉及环境检测、荧光传感等领域，具体涉及一种基于铋基钙钛矿量子点荧光传感器的制备方法及其应用。
背景技术
随着工业生产的不断发展，废弃污染物的不合理排放，造成的重金属污染已日趋严重，逐渐成为威胁人类生存与健康的环境问题。其中，Cr(Ⅵ)具有强毒性，极易通过空气、食物、水和土壤等环境进入人体，不仅会引起肝脏、肾脏等脏器损伤，还具有强致癌性，对人体健康造成了严重损伤。因此，实现Cr(Ⅵ)污染的检测对维护生态平衡以及人类自身健康具有重要意义。与电感耦合等离子质谱法、原子吸收分光光度法等检测方法相比，荧光传感法具有操作简单、灵敏度高、选择性好等优点，受到人们广泛关注。
钙钛矿量子点是一种新型光致发光材料，与传统的发光材料相比，具有荧光寿命长、颜色纯度高的优点，在传感器领域中有广泛的应用前景。其中，相对铅基、锡基等钙钛矿量子点而言，铋基钙钛矿量子点毒性低、稳定性强，在太阳能电池和光催化等领域中应用广泛，但较低的量子产率和仍需提高的稳定性限制了其进一步发展。
发明内容
本发明的目的是克服现有Cr(Ⅵ)检测技术操作复杂、灵敏度低等缺点，将铋基钙钛矿量子点应用于Cr(Ⅵ)检测，提供一种视觉可见、操作简单、高灵敏性的Cr(Ⅵ)检测方法。
本发明所采用的技术方案为：
一种基于铋基钙钛矿量子点荧光传感器的制备方法，由以下步骤实现,以下均以干质量份计：
1)取0.430-0.438份的氯化铯和0.608-0.616份的氯化铋放入20mL丝口瓶中，再加入0.259-0.271份二甲基亚砜、1.82-1.90份的壳聚糖和18.95-19.15份的1-烯丙基-3-甲基-卤化咪唑混合，50-80℃下搅拌10-30min形成前驱体溶液；
2)取0.5mL前驱体溶液，缓慢滴加到40.15-40.35份的无水乙醇和1.357-1.369份的油酸中，70-90℃下剧烈搅拌，反应10-30min，8000r/min离心，去除沉淀，得到[AMIM]Cl/CS-Cs3Bi2Cl9量子点荧光传感器。
进一步地，应用该荧光传感器进行Cr(Ⅵ)的识别和检测，具体方法为：将待测样品溶液加入所得荧光传感器中，然后在紫外灯下观察溶液的荧光淬灭情况，当溶液未出现荧光淬灭，则待测样品溶液中不含Cr(Ⅵ)，当溶液出现荧光淬灭，则待测样品溶液中含有Cr(Ⅵ)；
对Cr(Ⅵ)的线性检测范围是20-500μM，检测限为9μM。
进一步地，在365nm紫外灯下观察溶液荧光颜色的变化。
进一步地，将所得荧光传感器加入Cr(Ⅵ)浓度为0.01-2mM的水溶液，静置1-15min，检测其荧光强度做标准曲线，进而得到检测限及线性检测范围。
进一步地，所述荧光检测的激发波长为370nm,发射波长为440nm。
本发明具有以下优点：
1、本发明是一种基于铋基钙钛矿量子点荧光传感器检测水溶液中Cr(Ⅵ)的方法，对Cr(Ⅵ)的线性检测范围是20-500μM，检测限为9μM，在检测水环境中Cr(Ⅵ)的有很大的应用前景。
2、本发明制备的铋基钙钛矿量子点荧光传感器可以在水溶液中稳定存在，其表面的氨基和羟基可以与Cr(Ⅵ)进行结合，造成荧光强度的变化，进而实现对Cr(Ⅵ)的定量的检测和识别。
3、本发明利用生物质材料壳聚糖作为配体钝化铋基钙钛矿量子点，增强环境稳定性，提升量子产率，制备方法简单易行，成本低廉。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1：
一种基于铋基钙钛矿量子点荧光传感器的制备方法，由以下步骤实现,以下均以干质量份计：
1)取0.430份的氯化铯和0.608份的氯化铋放入20mL丝口瓶中，再加入0.259份二甲基亚砜、1.82份的壳聚糖和18.95份的1-烯丙基-3-甲基-氯化咪唑混合60℃下搅拌10min形成前驱体溶液；
2)取5mL前驱体溶液，缓慢滴加到40.15份的无水乙醇和1.357份的油酸中，80℃下剧烈搅拌，反应10min，自然冷却至室温，8000r/min离心，去除沉淀获得得到[AMIM]Cl/CS-Cs3Bi2Cl9量子点荧光传感器。
实施例2：
一种基于铋基钙钛矿量子点荧光传感器的制备方法，由以下步骤实现,以下均以干质量份计：
1)取0.434份的氯化铯和0.612份的氯化铋放入20mL丝口瓶中，再加入0.265份二甲基亚砜、1.86份的壳聚糖和19.05份的1-烯丙基-3-甲基-氯化咪唑混合，60℃下搅拌10min形成前驱体溶液；
2)取出5mL前驱体溶液，缓慢滴加到40.25份的无水乙醇和1.363份的油酸中，80℃下剧烈搅拌，反应10min，自然冷却至室温，8000r/min离心，去除沉淀获得[AMIM]Cl/CS-Cs3Bi2Cl9量子点荧光传感器。
实施例3：
一种基于铋基钙钛矿量子点荧光传感器的制备方法，由以下步骤实现,以下均以干质量份计：
1)取0.438份的氯化铯和0.616份的氯化铋放入20mL丝口瓶中，再加入0.271份二甲基亚砜、1.90份的壳聚糖和19.15份的1-烯丙基-3-甲基-氯化咪唑混合，60℃下搅拌10min形成前驱体溶液；
2)取出5mL前驱体溶液，缓慢滴加到40.35份的无水乙醇和1.369份的油酸中，80℃下剧烈搅拌，反应10min，自然冷却至室温，8000r/min离心，去除沉淀获得得到[AMIM]Cl/CS-Cs3Bi2Cl9量子点荧光传感器。
实施例4：
应用上述实施例中制得的荧光传感器进行Cr(Ⅵ)的识别和检测，具体方法为：将所得荧光传感器加入Cr(Ⅵ)浓度为0.01-2mM的水溶液，静置1-15min，检测其荧光强度做标准曲线，进而得到检测限及线性检测范围
将待测样品溶液加入所得荧光传感器中，然后在365nm的紫外灯下观察溶液的荧光淬灭情况，当溶液未出现荧光淬灭，则待测样品溶液中不含Cr(Ⅵ)，当溶液出现荧光淬灭，则待测样品溶液中含有Cr(Ⅵ)；得到对Cr(Ⅵ)的线性检测范围是20-500μM，线性相关方程为y＝2.489c(Cr(Ⅵ))+0.149，线性相关系数为0.98603，检测限为9μM。所述荧光检测的激发波长为370nm,发射波长为440nm。
为评价本发明方法的特异性，选取水溶液中常见的离子如Cu2+、Al3+、Mg2+、Cr3+，Cl-、NO3 -，按照上述的检测步骤对这些离子进行测定，记录各自的荧光强度并进行比较。结果表明，其他离子几乎不会引起传感器荧光强度的变化，这说明基于铋基钙钛矿量子点荧光传感器检测Cr(Ⅵ)的方法具有高度选择性。
Claims (5)
1.一种基于铋基钙钛矿量子点荧光传感器的制备方法，其特征在于，由以下步骤实现,以下均以干质量份计：
1)取0.430-0.438份的氯化铯和0.608-0.616份的氯化铋放入20mL丝口瓶中，再加入0.259-0.271份二甲基亚砜、1.82-1.90份的壳聚糖和18.95-19.15份的1-烯丙基-3-甲基-卤化咪唑混合，50-80℃下搅拌10-30min形成前驱体溶液；
2)取0.5mL前驱体溶液，缓慢滴加到40.15-40.35份的无水乙醇和1.357-1.369份的油酸中，70-90℃下剧烈搅拌，反应10-30min，8000r/min离心，去除沉淀，得到[AMIM]Cl/CS-Cs3Bi2Cl9量子点荧光传感器。
2.根据权利要求1所述方法制备得到的荧光传感器的应用，其特征在于：
应用该荧光传感器进行Cr(Ⅵ)的识别和检测，具体方法为：将待测样品溶液加入所得荧光传感器中，然后在紫外灯下观察溶液的荧光淬灭情况，当溶液未出现荧光淬灭，则待测样品溶液中不含Cr(Ⅵ)，当溶液出现荧光淬灭，则待测样品溶液中含有Cr(Ⅵ)；
对Cr(Ⅵ)的线性检测范围是20-500μM，检测限为9μM。
3.根据权利要求2所述的荧光传感器的应用，其特征在于：在365nm紫外灯下观察溶液荧光颜色的变化。
4.根据权利要求3所述的荧光传感器的应用，其特征在于：将所得荧光传感器加入Cr(Ⅵ)浓度为0.01-2mM的水溶液，静置1-15min，检测其荧光强度做标准曲线，进而得到检测限及线性检测范围。
5.根据权利要求4所述的荧光传感器的应用，其特征在于，所述荧光检测的激发波长为370nm,发射波长为440nm。
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