CN114907845A - 一种三基色荧光碳量子点及其制备方法和应用 - Google Patents
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Abstract
本发明属于碳量子点技术领域,具体涉及一种三基色荧光碳量子点及其制备方法和应用。制备方法如下:将邻苯二胺和不同量的硝酸溶于水中,超声,形成均匀分散的混合溶液;将所得混合溶液转移到聚四氟乙烯高压反应釜中,再将反应釜转移到烘箱中,进行水热反应;将所得反应溶液离心,透析,冷冻干燥,得到三种不同颜色荧光碳量子点,分别为红色、绿色、蓝色。CDs的全色发光行为在固体聚合物基质中继承和保守,得到了多色CDs/聚合物薄膜,并且将近红外的R‑CDs制备成pH检测试纸,在紫外灯和日光灯下以比色的方式在超宽范围内去检测溶液的pH,建立了一种新型的比色双模pH检测系统。
Description
技术领域
本发明属于碳量子点技术领域,具体涉及一种三基色荧光碳量子点及其制备方法和应用。
背景技术
碳点(CDs)具有低毒、高光稳定性、在各种溶剂中具有良好的分散性、生物相容性、具有良好的光致发光(PL)性能等优点,是近年来被广泛研究的一种优良的多功能材料。多色发光材料因其在传感、生物成像、全色显示、发光二极管和光电子器件等方面的广泛应用而备受关注。因此,开发高实用性和丰富的色彩调节的新型多色发光材料仍然是一个挑战。
参考传统pH试纸的成功应用,研究人员开发了如此多的视觉荧光试纸,可以通过紫外日光双模比色策略用肉眼对样品进行定性分析。荧光材料的光学pH传感器具有灵敏度高、直观(肉眼)观察等优点。光学pH传感器基于有机染料、半导体量子点、纳米粒子和荧光蛋白。然而,半导体量子点和蛋白质通常需要多步骤、复杂的制备过程。基于聚合物和小分子的传感器通常没有足够的光学或热稳定性,而且通常是有毒的,这限制了应用。因此,开发稳定的、环境友好的材料,使用比色双模法来测定超宽范围内的pH值是非常重要的。
尽管前人在传统pH试纸上已经做了很多工作,但是基于近红外CDs的传感器进行双模比色检测超宽范围内的pH响应还尚未报道。目前,简易制备三基色碳点并应用于荧光薄膜,具有近红外发光碳点用于比色双模式下用于超宽范围内的pH检测的碳量子点体系还未见报道。
发明内容
为了解决以上问题,本发明的目的是,利用邻苯二胺和不同量的硝酸,一锅水热法制备三色发光的荧光碳量子点基探针,并将荧光碳量子点应用于多色有机薄膜的制备以及比色双模式下超宽范围的pH检测。
本发明采用的技术方案是:一种三基色荧光碳量子点,制备方法包括如下步骤:
1)将邻苯二胺和不同质量的硝酸溶于水中,超声,形成均匀分散的混合溶液;
2)将所得混合溶液转移高压反应釜中,再将反应釜转移到烘箱中,进行水热反应;
3)将步骤2)所得反应溶液离心,透析;
4)将步骤3)所得产物,冷冻干燥,得到三种不同颜色荧光碳量子点,分别为红色、绿色、蓝色。
优选地,上述的一种三基色荧光碳量子点,步骤1)中,按固液比,邻苯二胺:硝酸=3g:0-2.6mL。
优选地,上述的一种三基色荧光碳量子点,步骤2)中,所述水热反应是,于180℃下反应12h。
优选地,上述的一种三基色荧光碳量子点,步骤3)中,所述离心是,转速为8000r/min下离心5min。
优选地,上述的一种三基色荧光碳量子点,步骤3)中,所述透析是,透析袋截留分子量为500D,透析时间为48h。
上述的一种三基色荧光碳量子点在制备多色有机薄膜中的应用。
优选地,上述的应用,多色有机薄膜的制备方法包括如下步骤:将上述的任一种三基色荧光碳量子点的乙醇溶液加入到5%PVA溶液中,得到CDs/PVA混合溶液,将CDs/PVA混合溶液涂在玻璃上,在45℃下模压48h后得到CDs/PVA薄膜。
上述的一种三基色荧光碳量子点在检测pH中的应用。
优选地,上述的应用,将滤纸片浸泡在上述三基色荧光碳量子点的溶液中,取出滤纸干燥后,将不同pH的缓冲溶液滴在滤纸上,在日光灯下观察滤纸颜色变化。
本发明的有益效果是:
1、本发明中,邻苯二胺含有苯环结构,通过水热法形成荧光碳量子点,因为加入的硝酸含量不同,进一步制成不同发射的荧光碳量子点。本发明制备的三色荧光碳量子点,其制备方法简单,安全,原料廉价易得,适合大批量生产。
2、本发明制备得到的三种发射的荧光碳量子点,其三色CDs的发光行为在固体聚合物基质中继承和保守,因此选择PVP有机溶液制备得到了多色CDs/PVP聚合物薄膜。
3、本发明提供的荧光碳量子点基探针,可以在紫外和日光灯双模式下进行检测pH的方法,具有较宽范围的pH检测范围,具有很大的应用前景。
附图说明
图1a-c是分别是B-CDs、G-CDs、R-CDs的透射电镜图。
图2是分别是B-CDs、G-CDs、R-CDs在的乙醇溶剂中的光致发光光谱图。
图3是三色荧光碳量子点的紫外吸收峰。
图4是三色荧光碳量子点色坐标。
图5是三色荧光碳量子点基荧光碳量子点基探针的红外谱图。
图6是在365nm紫外光激发下具有多色发光的CDS/PVA薄膜。
图7a是用R-CDs制备得到的CDs滤纸检测pH在日光下的成像。
图7b是用R-CDs制备得到的CDs滤纸检测pH在紫外灯UV365nm下的成像。
具体实施方式
为了更好地理解本发明,下面通过实施例对本发明做进一步说明,应理解以下实施目的在于更好地解释本发明的内容,而不是对本发明的保护范围产生任何限制。
实施例1荧光碳量子点基探针(一)制备方法包括如下步骤:
1)将0.24mL、0mL、0.26mL 12mol/L硝酸分别溶于10mL水中,将三份0.3g的邻苯二胺分别加入到上述溶液中,超声15min,分别得到三种均匀分散的混合溶液;
2)将步骤1)所得三种混合溶液分别转移到聚四氟乙烯高压反应釜中,再将反应釜转移到烘箱中,180℃下水热反应12h,得反应溶液;
3)将步骤2)所得三种反应溶液,在转速为8000r/min下,离心5min,取上清液用500D的透析袋透析48h;
4)将步骤3)所得三种产物透析后的产物,在冷冻干燥机中冷冻干燥48h,得B-CDs、G-CDs、R-CDs固态粉末。分别为蓝色荧光碳点、绿色荧光碳点、红色荧光碳点。
(二)检测
图1a-图1c是荧光碳量子点基探针的透射电镜图。B-CDs、G-CDs、R-CDs荧光碳量子基探针在乙醇溶液中均匀分散,且B-CDs平均直径为2.5nm、G-CDs平均直径为3.7nm、R-CDs平均直径为4nm,且插图显示出其都具有0.21nm晶格间距,为石墨烯(100)面。
图2是显示的是B-CDs、G-CDs、R-CDs在乙醇溶剂中的荧光激发和发射光谱图。从图中可以看出B-CDs、G-CDs、R-CDs在最佳激发波长下的奖最佳发射位置分别为400nm、550nm、610nm。图4是三色荧光碳量子点色坐标。
图3是三色荧光碳量子点的紫外吸收峰。由图可见,284nm处吸收代表π-π*跃迁,534nm和578nm处的吸收代表n-π*跃迁。在210~350nm的紫外区,在345nm处观察到单峰,肩峰位于282nm,分别对应于C=O键的n-π*跃迁和C=N键的π-π*跃迁.随着制备温度的升高,n-π*峰降低,而π-π*峰升高。π-π*跃迁的升高表明π-π*态之间的能隙增加,以及共轭sp2结构域的增加。
图5是邻苯二胺和荧光碳量子点基探针的红外谱图,各处峰分别代表基团:N-H(3430cm-1),C=N/C=C(1602cm-1),C-N(1499and 1350cm-1),C-O(1110cm-1)。
实施例2一种基于三色荧光碳量子点制备的CDs/PVA薄膜
方法:一种简单的方法制备了CDs/PVA薄膜,首先在95℃下将5g PVA分散于95g去离子水中,制得5%PVA溶液,然后将浓度分别为0.01、0.05、0.15、0.25mg/mL的1mLCDs乙醇溶液加入9mL 5%PVA溶液中。将CDs/PVA混合溶液涂在一块光滑的玻璃上。在45℃下模压48h后,测试CDs/PVA薄膜的荧光光谱。
图6显示成功地制备了全色发光的CDs/聚乙烯醇(PVA)复合薄膜。其薄膜在紫外灯下显示出清晰的蓝、绿、红三色的有薄膜,其荧光性质也基本上没有大的差别,并且能够稳定存在。
实施例3一种三基色荧光碳量子点在检测pH中的应用
方法:将已经剪好的滤纸片(大小为1*1cm)浸泡在0.01mol/L的R-CDs溶液中,待滤纸风干后,将不同pH为1、2、4、6、7、8、9、11、13的缓冲溶液滴在滤纸上,在日光灯下观察滤纸颜色变化。
图7是日光下R-CDs荧光碳量子点在不同pH的条件下的颜色变化图。将不同pH为1、2、4、6、7、8、9、11、13的缓冲溶液滴在滤纸上,在日光灯下观察滤纸颜色变化为酸性环境下的蓝色逐渐转变为中性环境下红色,粉红色,最后在碱性环境中为橙黄色,颜色突跃较为明显,在紫外灯下UV(365nm)照射下其颜色也可以发生较为明显的改变,这个方法进行了pH的双模检测,是个很不错的pH检测方法。
Claims (9)
1.一种三基色荧光碳量子点,其特征在于:制备方法包括如下步骤:
1)将邻苯二胺和不同质量的硝酸溶于水中,超声,形成均匀分散的混合溶液;
2)将所得混合溶液转移高压反应釜中,再将反应釜转移到烘箱中,进行水热反应;
3)将步骤2)所得反应溶液离心,透析;
4)将步骤3)所得产物,冷冻干燥,得到三种不同颜色荧光碳量子点,分别为红色、绿色、蓝色。
2.根据权利要求1所述的一种三基色荧光碳量子点,其特征在于:步骤1)中,按固液比,邻苯二胺:硝酸=3g:0-2.6mL,所述的硝酸的浓度为12mol/L。
3.根据权利要求1所述的一种三基色荧光碳量子点,其特征在于:步骤2)中,所述水热反应是,于180℃下反应12h。
4.根据权利要求1所述的一种三基色荧光碳量子点,其特征在于:步骤3)中,所述离心是,转速为8000r/min下离心5min。
5.根据权利要求1所述的一种三基色荧光碳量子点,其特征在于:步骤3)中,所述透析是,透析袋截留分子量为500D,透析时间为48h。
6.权利要求1-5任意一项所述的一种三基色荧光碳量子点在制备多色有机薄膜中的应用。
7.根据权利要求6所述的应用,其特征在于:多色有机薄膜的制备方法包括如下步骤:将权利要求1-5所述的任一种三基色荧光碳量子点的乙醇溶液加入到5%PVA溶液中,得到CDs/PVA混合溶液,将CDs/PVA混合溶液涂在玻璃上,在45℃下模压48h后得到CDs/PVA薄膜。
8.权利要求1-5任意一项所述的一种三基色荧光碳量子点在检测pH中的应用。
9.根据权利要去8所述的应用,其特征在于,将滤纸片浸泡在权利要求1-5任意一项所述三基色荧光碳量子点的溶液中,取出滤纸干燥后,将不同pH的缓冲溶液滴在滤纸上,在日光灯下观察滤纸颜色变化。
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