CN110437835B - 一种硫化铈掺杂碳量子点纳米荧光材料的制备方法 - Google Patents
一种硫化铈掺杂碳量子点纳米荧光材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种硫化铈掺杂碳量子点纳米荧光材料的制备方法,其特征在于,采用去离子水,衣康酸,三氯化铈,配制得到A液;去离子水,硫代乙酰胺,配制得到B液;然后,在反应器中加入A液搅拌,将B液滴加到A液中,A液与B液的体积比为5:1,滴加完毕,搅拌反应30min,转移到反应釜中,盖好密封盖,置于恒温箱中,温度在180±2℃恒温,反应20~24h,得到红色悬浊液体,固液分离,液体为粗品硫化铈掺杂碳量子点纳米荧光材料;采用透析法提纯硫化铈掺杂碳量子点纳米荧光材料。该制备方法具有绿色环保,操作简单,硫化铈掺杂碳量子点纳米荧光材料不需要二次修饰既可以具有荧光性能稳定性高、尺寸小而均匀,生物相容性好等特点。
Description
技术领域
本发明属于纳米发光材料制备技术领域,特别涉及一种硫化铈掺杂碳量子点纳米荧光材料的制备方法及荧光性能。
背景技术
碳量子点作为一种新兴的纳米材料,碳量子点(C-Dots)具有生物兼容性好且无毒、粒径小、发射光谱可调、荧光稳定性高且耐光漂白等优点,加之原料廉价且来源丰富、易于制备和修饰等特点,使其制备和应用成为近年来分析化学的热点研究领域之一。然而,目前有关荧光C-Dots纳米材料的研究还处于初期阶段,仍存在一些亟待解决的科研问题,如现有合成方法的产量和荧光量子产率(QY)往往比较低,无法准确控制其横向尺寸及表面化学、发光机制不明确、荧光光谱范围窄等。因此,该研究领域还存在巨大的发展空间。
碳量子点除自身具有广泛应用外,基于碳量子点复合材料的研究也是目前的热点课题。复合材料是由两种或两种以上的不同材料复合而成,每种组成材料相互协同,不仅发挥各自的优势,还可拥有新的性能。因此,基于碳量子点复合材料的研究是碳量子点功能化的一个重要课题。碳量子点是以碳为骨架结构的纳米材料,是一种分散的、尺寸小于10nm的类球形纳米颗粒,一般包括纳米金刚石、碳颗粒和石墨烯量子点,也称碳点、碳纳米点、碳纳米晶。碳量子点是荧光碳纳米材料中最重要的一种,它具有独特的小尺寸特性和优越的荧光性质;碳量子点荧光明亮、稳定,激发光谱宽,发射光谱窄,且发射波长可通过改变材料的粒径大小和组成来调控,无光漂白现象,某些碳量子点还有,上转换荧光特性。杂原子的掺杂可以提高碳量子的荧光产率,以促进碳量子点在生物医学领域得以发展和应用,选择有机自然生物作碳源合成碳量子点更可取。
稀土元素的原子具有未充满的受到外界屏蔽的4f5d电子组态,因此有丰富的电子能级和长寿命激发态,能级跃迁通道多达20余万个,可以产生多种多样的辐射吸收和发射,构成广泛的发光和激光材料。随着稀土分离、提纯技术的进步,以及相关技术的促进,稀土发光材料的研究和应用得到显著发展。发光是稀土化合物光、电、磁三大功能中最突出的功能,受到人们极大的关注。将不同稀土元素化合物掺杂到碳量子点中,对其光学性能具有显著改善。
硫化铈为红色粉状物质偏黄相无机颜料,铈为稀土中所含17种重要元素之一,硫化铈为红色粉状物质偏黄相无机颜料,含有稀土成份,硫化铈红使用在各种材质上具有荧光艳丽的红色效果,采用硫化铈掺杂碳量子点,可得到粉红色的碳量子点,荧光的发射波长在540nm,其吸收光谱的最大波长在510nm左右,也可用于可见光波长范围的分光测定。
本申请以衣康酸为碳源,以硫代乙酰胺为均相硫源,氯化铈为铈源,采用水热方法制备一种硫化铈掺杂碳量子点纳米荧光材料。
发明内容
本发明的目的在于提供一种硫化铈掺杂碳量子点纳米荧光材料的制备方法。
一种硫化铈掺杂碳量子点纳米荧光材料的制备方法,其特征在于,该方法具有以下工艺步骤:
(1)A液配制:在反应器中,按如下组成质量百分比加入,去离子水:62~66%,衣康酸:32~36%,三氯化铈:1.5~2.5%,各组分之和为百分之百,搅拌溶解,得到A液;
(2)B液配制:在反应器中,按如下组成质量百分比加入,去离子水:92~94%,硫代乙酰胺:6.0~8.0%,各组分之和为百分之百,搅拌溶解,得到B液;
(3)粗品硫化铈掺杂碳量子点纳米荧光材料的制备:在反应器中加入A液搅拌,将B液滴加到A液中,A液与B液的体积比为5:1,滴加完毕,搅拌反应30min,转移到反应釜中,盖好密封盖,置于恒温箱中,温度在180±2℃恒温,反应20~24h,得到红色悬浊液体,固液分离,液体为粗品硫化铈掺杂碳量子点纳米荧光材料;
(4)硫化铈掺杂碳量子点纳米荧光材料的提纯:将步骤(3)得到的液体注入到透析袋内进行透析,其截留分子量为800D,透析时间为30h,每间隔4h换一次水;将透析产物进行蒸发,得到浓缩溶液;干燥至粉末状,获得硫化铈掺杂碳量子点纳米荧光材料。
在步骤(1)中所述的三氯化铈为含有7个结晶水的三氯化铈。
所述的三氯化铈与硫代乙酰胺的摩尔比为1:3。
所制备的硫化铈掺杂碳量子点纳米荧光材料的荧光量子产率为35.12%,量子产率高。在波长390nm的激发波长下,能成功发射出的荧光(510nm)。
本发明的有益效果是:
本申请采用硫代乙酰胺和三氯化铈为掺杂硫化铈源,衣康酸为碳源,采用水热法合成硫化铈掺杂碳量子点纳米荧光材料,该方法具有绿色环保,操作简单,均相反应,所制备的硫化铈掺杂碳量子点纳米荧光材料不需要二次修饰既可以具有荧光性能稳定性高、尺寸小而均匀,生物相容性好等特点,硫化铈掺杂碳量子点纳米荧光材料的荧光性能(量子产率)可提高近250%。
附图说明
图1为本申请所制备的硫化铈掺杂碳量子点纳米荧光材料的透射电镜图。
图2为本申请所制备的硫化铈掺杂碳量子点纳米荧光材料的荧光激发和发射光谱图;图中曲线1为激发光谱,曲线2为发射光谱。
具体实施方式
实施例1
(1)A液配制:在反应器中,分别加入,去离子水:64mL,衣康酸:34g,三氯化铈:2g,搅拌溶解,得到A液;
(2)B液配制:在反应器中,分别加入,去离子水:93mL,硫代乙酰胺:7g,搅拌溶解,得到B液;
(3)粗品硫化铈掺杂碳量子点纳米荧光材料的制备:在反应器中加入A液:50mL,搅拌,滴加B液:10mL到A液中,滴加完毕,搅拌反应30min,转移到反应釜中,盖好密封盖,置于恒温箱中,温度在180±2℃恒温,反应22h,得到红色悬浊液体,固液分离,液体为粗品硫化铈掺杂碳量子点纳米荧光材料;
(4)硫化铈掺杂碳量子点纳米荧光材料的提纯:将步骤(3)得到的液体注入到透析袋内进行透析,其截留分子量为800D,透析时间为30h,每间隔4h换一次水;将透析产物进行蒸发,得到浓缩溶液;干燥至粉末状,获得硫化铈掺杂碳量子点纳米荧光材料。
实施例2
(1)A液配制:在反应器中,分别加入,去离子水:62mL,衣康酸:35.5g,三氯化铈:2.5g,搅拌溶解,得到A液;
(2)B液配制:在反应器中,分别加入,去离子水:92mL,硫代乙酰胺:8g,搅拌溶解,得到B液;
(3)粗品硫化铈掺杂碳量子点纳米荧光材料的制备:在反应器中加入A液:100mL,搅拌,滴加B液:20mL到A液中,滴加完毕,搅拌反应30min,转移到反应釜中,盖好密封盖,置于恒温箱中,温度在180±2℃恒温,反应20h,得到红色悬浊液体,固液分离,液体为粗品硫化铈掺杂碳量子点纳米荧光材料;
(4)硫化铈掺杂碳量子点纳米荧光材料的提纯:将步骤(3)得到的液体注入到透析袋内进行透析,其截留分子量为800D,透析时间为30h,每间隔4h换一次水;将透析产物进行蒸发,得到浓缩溶液;干燥至粉末状,获得硫化铈掺杂碳量子点纳米荧光材料。
实施例3
(1)A液配制:在反应器中,分别加入,去离子水:66mL,衣康酸:32.5g,三氯化铈:1.5g,搅拌溶解,得到A液;
(2)B液配制:在反应器中,分别加入,去离子水:94mL,硫代乙酰胺:6g,搅拌溶解,得到B液;
(3)粗品硫化铈掺杂碳量子点纳米荧光材料的制备:在反应器中加入A液:150mL,搅拌,滴加B液:30mL到A液中,滴加完毕,搅拌反应30min,转移到反应釜中,盖好密封盖,置于恒温箱中,温度在180±2℃恒温,反应24h,得到红色悬浊液体,固液分离,液体为粗品硫化铈掺杂碳量子点纳米荧光材料;
(4)硫化铈掺杂碳量子点纳米荧光材料的提纯:将步骤(3)得到的液体注入到透析袋内进行透析,其截留分子量为800D,透析时间为30h,每间隔4h换一次水;将透析产物进行蒸发,得到浓缩溶液;干燥至粉末状,获得硫化铈掺杂碳量子点纳米荧光材料。
硫化铈掺杂碳量子点纳米荧光材料荧光产率的测量:选择了参比法:选择稀硫酸为溶剂,将硫酸奎宁溶解在0.1mol/LH2SO4溶液中(可以增加硫酸奎宁的溶解度)形成硫酸奎宁的酸溶液,然后于紫外可见分光光度计中测量碳量子点和硫酸奎宁酸溶液在固定激发波长处的吸光度。最后于荧光光谱仪中测量碳量子点和硫酸奎宁酸溶液在给定激发波长下的荧光发射光谱图,得到荧光积分面积。按照公式计算荧光量子产率:
Claims (3)
1.一种硫化铈掺杂碳量子点纳米荧光材料的制备方法,其特征在于,该方法具有以下工艺步骤:
(1)A液配制:在反应器中,按如下组成质量百分比加入,去离子水:62~66%,衣康酸:32~36%,三氯化铈:1.5~2.5%,各组分之和为百分之百,搅拌溶解,得到A液;
(2)B液配制:在反应器中,按如下组成质量百分比加入,去离子水:92~94%,硫代乙酰胺:6.0~8.0%,各组分之和为百分之百,搅拌溶解,得到B液;
(3)粗品硫化铈掺杂碳量子点纳米荧光材料的制备:在反应器中加入A液搅拌,将B液滴加到A液中,A液与B液的体积比为5:1,滴加完毕,搅拌反应30min,转移到反应釜中,盖好密封盖,置于恒温箱中,温度在180±2℃恒温,反应20~24h,得到红色悬浊液体,固液分离,液体为粗品硫化铈掺杂碳量子点纳米荧光材料;
(4)硫化铈掺杂碳量子点纳米荧光材料的提纯:将步骤(3)得到的液体注入到透析袋内进行透析,其截留分子量为800D,透析时间为30h,每间隔4h换一次水;将透析产物进行蒸发,得到浓缩溶液;干燥至粉末状,获得硫化铈掺杂碳量子点纳米荧光材料。
2.根据权利要求1所述的一种硫化铈掺杂碳量子点纳米荧光材料的制备方法,其特征在于,步骤(1)中所述的三氯化铈为含有7个结晶水的三氯化铈。
3.根据权利要求1所述的一种硫化铈掺杂碳量子点纳米荧光材料的制备方法,其特征在于,所述的三氯化铈与硫代乙酰胺的摩尔比为1:3。
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Aptamer-mediated N/Ce-doped carbon dots as a fluorescent and resonance Rayleigh scattering dual mode probe for arsenic(III);Zhang Zhihao;《MICROCHIMICA ACTA》;20190822;第186卷(第9期);全文 * |
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