CN105542763A - 一种用碳量子点制备单一基质荧光膜的方法 - Google Patents
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Abstract
本发明涉及一种用碳量子点制备单一基质荧光膜的方法,是针对白光发光二极管实现白光的特点,以柠檬酸、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷为原料,经水热合成、滤膜过滤、透析、成膜,制成碳量子点单一基质荧光膜,并用以制备白光发光二极管,此制备方法工艺先进,数据精确翔实,制备的碳量子点单一基质荧光膜膜层厚度≤100nm,纯度达99.8%,膜层均匀,可用于发光二极管合成白光,是十分先进的用碳量子点制备单一基质荧光膜的方法。
Description
技术领域
本发明涉及一种用碳量子点制备单一基质荧光膜的方法,属光致发光材料制备及应用的技术领域。
背景技术
固态的发光二极管LED具有能效高、寿命长、能耗低的特点,是新一代发光光源。
白光发光二极管实现白光主要有三种形式,一种是蓝光芯片加黄色荧光粉,二是紫外芯片加红绿蓝荧光粉,三是紫外光芯片加单一基质荧光粉;常用的方法是蓝光芯片加黄色荧光粉,这一方法实现白光简单,但由于荧光粉在红光区域发射较弱,致使发光二极管显色指数低;紫外芯片和红绿蓝荧光粉合成白光,但由于复合的荧光粉存在严重的颜色重吸收问题,而导致器件效率的损失;稀土类荧光粉做单一基质荧光粉可做白光发光器件,但稀土类荧光粉价格昂贵,不利于大量推广;单一基质的半导体量子点也可做白光发光器件荧光粉,但由于含有有毒元素而限制了其广泛应用。
荧光碳量子点是一种尺寸≤10nm的量子点,具有优越的光学性质、低毒,且具有生物兼容性,高的化学惰性,是单一基质荧光膜的优选材料,此项技术还处于研究阶段。
发明内容
发明目的
本发明的目的是针对背景技术的状况,以柠檬酸,N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷为原料,经水热合成、滤膜过滤、透析袋透析、成膜,制成碳量子点单一基质荧光膜,以用于制备白光二极管。
技术方案
本发明使用的化学物质材料为:柠檬酸、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷、去离子水、导电玻璃,其组合准备用量如下:以克、毫升、毫米为计量单位
制备方法如下:
(1)精选化学物质材料
对制备使用的化学物质材料要进行精选,并进行质量纯度控制:
柠檬酸:固态固体99.9%
N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷:液态液体99.9%
去离子水:液态液体99.9%
导电玻璃:固态固体
(2)水热合成制备碳量子点水溶液
①配制混合溶液
在聚四氟乙烯容器中,加入柠檬酸1.05g±0.001g、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷21.63mL±0.001mL、去离子水40mL±0.001mL,搅拌5min,使其溶解,成混合溶液;
②将装有混合溶液的聚四氟乙烯容器置于超声波分散仪中,进行超声分散,超声波频率60KHz,超声分散时间10min;
③超声分散后,将盛有混合溶液的聚四氟乙烯容器置于反应釜中,并密闭;
④将反应釜置于电加热炉中,进行加热,加热温度200℃±1℃、加热时间360min;
混合溶液在反应釜内,在水热合成过程中将发生化学反应,反应方程式如下:
式中:CDs:碳量子点
⑤冷却,水热合成后停止加热,混合溶液随加热炉反应釜冷却至25℃;
(3)过滤
将冷却后的混合溶液置于烧杯中,用注射器吸取溶液,用0.22mm的微孔滤膜进行过滤,留存滤液,弃掉滤膜及其上的沉淀物;
(4)透析
①将滤液置于纤维素透析袋内,并密闭;
②将盛有滤液的纤维素透析袋置于烧杯中,加入去离子水800mL,去离子水要淹没纤维素透析袋,在烧杯底部置放磁子搅拌器;
③将烧杯置于电加热器上,加热温度30℃±1℃,磁子搅拌器搅拌,加热搅拌时间9h;
④透析后,停止加热,停止搅拌,使纤维素透析袋内的滤液冷却至25℃;
(5)成膜
①预处理导电玻璃
将导电玻璃置于烧杯中,加入去离子水200mL,浸泡洗涤30min;
浸泡后,将导电玻璃取出,垂直吊装在不锈钢支架上,然后置于真空干燥箱中干燥,干燥温度80℃,真空度8Pa,干燥时间30min;
②将干燥后的导电玻璃平面置于石英板上,将纤维素透析袋内的滤液均匀置于导电玻璃上;
③真空干燥
将导电玻璃置于真空干燥箱中,进行干燥处理,干燥温度80℃,真空度6Pa,干燥时间120min;
干燥后为碳量子点单一基质荧光膜;
(6)检测、分析、表征
对制备的碳量子点单一基质荧光膜的形貌、色泽、纯度、化学物理性能、发光性能进行检测、分析、表征;
用透射电子显微镜进行形貌分析;
用荧光光谱仪和紫外可见分光光度计进行荧光性能分析;
用X射线衍射仪进行结构分析;
结论:碳量子点单一基质荧光膜为浅黄色薄膜,膜层厚度≤100nm,
产物纯度达99.8%;
(7)产物储存
将导电玻璃及其上的碳量子点单一基质荧光膜储存于棕色透明的玻璃容器内,密闭避光储存,要防晒、防潮、防酸碱盐侵蚀,储存温度20℃,相对湿度≤10%。
有益效果
本发明与背景技术相比具有明显的先进性,是针对白光发光二极管实现白光的特点,以柠檬酸、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷为原料,经水热合成,滤膜过滤、透析、成膜,制成碳量子点单一基质荧光膜,并用以制备白光二极管;此制备方法工艺先进,数据精确翔实,制备的碳量子点单一基质荧光膜膜层厚度≤100nm,纯度达99.8%,膜层均匀,可用于发光二极管合成白光,是十分先进的用碳量子点制备单一基质荧光膜的方法。
附图说明
图1、水热合成制备碳量子点溶液状态图
图2、发光二极管结构图
图3、碳量子点单一基质荧光膜形貌图
图4、碳量子点单一基质荧光膜X射线衍射图谱
图5、碳量子点单一基质荧光膜色坐标图
图中所示,附图标记清单如下:
1、加热炉,2、炉座,3、显示屏,4、指示灯,5、电源开关,6、加热温度控制器,7、反应釜,8、聚四氟乙烯容器,9、混合溶液,10、炉盖,11、釜盖,12、容器盖,13、工作台,14、发光二极管芯片座,15、固晶,16、第一导线,17、芯片,18、荧光粉,19、第一电极,20、第二电极,21、透镜,22、第二导线。
具体实施方式
以下结合附图对本发明做进一步说明:
图1所示,为制备碳量子点水热合成状态图,各部位置、连接关系要正确,按量配比,按序操作。
制备使用的化学物质的量值是按预先设置的范围确定的,以克、毫升、毫米为计量单位。
制备碳量子点水溶液是在反应釜内进行的,是在配制溶液、加热炉加热、水热合成过程中完成的;
加热炉为立式,加热炉1的下部为炉座2、上部为炉盖10,在加热炉1的内底部设有工作台13,在工作台13上部置放反应釜7,反应釜7上部为釜盖11,在反应釜7内置放聚四氟乙烯容器8,聚四氟乙烯容器8上部为容器盖12,在聚四氟乙烯容器8内为混合溶液9,并密闭;在炉座2上设有显示屏3、指示灯4、电源开关5、加热温度控制器6。
图2所示,为发光二极管结构图,发光二极管芯片座14为平面体,发光二极管芯片座14两侧设有第一电极19、第二电极20,发光二极管芯片座14上部为透镜21,透镜21内壁为荧光粉18,在发光二极管芯片座14上部为固晶15,固晶15上部为芯片17,在芯片17两侧设有第一导线16、第二导线22,第一导线16与第一电极19连接,第二导线22与第二电极20连接。
图3所示,为碳量子点单一基质荧光膜形貌图,碳量子点颗粒为球形,分散性好,无团聚现象,粒径分布范围较窄,粒径≦5nm。
图4所示,为碳量子点单一基质荧光膜X射线衍射图谱,图中所示,纵坐标为衍射强度、横坐标为衍射角2θ,碳量子点的馒头峰峰位在26°,表明制备的碳量子点中碳的石墨化程度较低,为无定形碳。
图5所示,为碳量子点单一基质荧光膜色坐标图,图中所示,色坐标为x=0.320,y=0.343,属白光区域。
实施例1
用碳量子点单一基质荧光膜制备白光发光二极管:
①配制单一基质碳量子点荧光膜水溶液
将导电玻璃及其上的荧光膜置于烧杯中,滴入去离子水8mL,然后置于加热器上,加热温度30℃,加热时间40min,使碳量子点单一基质荧光膜溶解,成荧光膜溶液;
②打开发光二极管芯片座14上的透镜21,将荧光膜溶液均匀滴入透镜内,滴入量为0.03mL;
③将滴入荧光膜溶液的透镜置于真空干燥箱中干燥,干燥温度80℃,真空度6Pa,干燥时间180min;
④干燥后,将发光二极管芯片座14上的透镜21封盖,并密闭,即完成了白光发光二极管的制备。
Claims (3)
1.一种用碳量子点制备单一基质荧光膜的方法,其特征在于:使用的化学物质材料为:柠檬酸、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷、去离子水、导电玻璃,其组合准备用量如下:以克、毫升、毫米为计量单位
制备方法如下:
(1)精选化学物质材料
对制备使用的化学物质材料要进行精选,并进行质量纯度控制:
柠檬酸:固态固体99.9%
N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷:液态液体99.9%
去离子水:液态液体99.9%
导电玻璃:固态固体
(2)水热合成制备碳量子点水溶液
①配制混合溶液
在聚四氟乙烯容器中,加入柠檬酸1.05g±0.001g、N-β-(氨乙基)-γ-氨丙基三甲氧基硅烷21.63mL±0.001mL、去离子水40mL±0.001mL,搅拌5min,使其溶解,成混合溶液;
②将装有混合溶液的聚四氟乙烯容器置于超声波分散仪中,进行超声分散,超声波频率60KHz,超声分散时间10min;
③超声分散后,将盛有混合溶液的聚四氟乙烯容器置于反应釜中,并密闭;
④将反应釜置于电加热炉中,进行加热,加热温度200℃±1℃、加热时间360min;
混合溶液在反应釜内,在水热合成过程中将发生化学反应,反应方程式如下:
式中:CDs:碳量子点
⑤冷却,水热合成后停止加热,混合溶液随加热炉反应釜冷却至25℃;
(3)过滤
将冷却后的混合溶液置于烧杯中,用注射器吸取溶液,用220μm的微孔滤膜进行过滤,留存滤液,弃掉滤膜及其上的沉淀物;
(4)透析
①将滤液置于纤维素透析袋内,并密闭;
②将盛有滤液的纤维素透析袋置于烧杯中,加入去离子水800mL,去离子水要淹没纤维素透析袋,在烧杯底部置放磁子搅拌器;
③将烧杯置于电加热器上,加热温度30℃±1℃,磁子搅拌器搅拌,加热搅拌时间9h;
④透析后,停止加热,停止搅拌,使纤维素透析袋内的滤液冷却至25℃;
(5)成膜
①预处理导电玻璃
将导电玻璃置于烧杯中,加入去离子水200mL,浸泡洗涤30min;
浸泡后,将导电玻璃取出,垂直吊装在不锈钢支架上,然后置于真空干燥箱中干燥,干燥温度80℃,真空度8Pa,干燥时间30min;
②将干燥后的导电玻璃平面置于石英板上,将纤维素透析袋内的滤液均匀置于导电玻璃上;
③真空干燥
将导电玻璃置于真空干燥箱中,进行干燥处理,干燥温度80℃,真空度6Pa,干燥时间120min;
干燥后为碳量子点单一基质荧光膜;
(6)检测、分析、表征
对制备的碳量子点单一基质荧光膜的形貌、色泽、纯度、化学物理性能、发光性能进行检测、分析、表征;
用透射电子显微镜进行形貌分析;
用荧光光谱仪和紫外可见分光光度计进行荧光性能分析;
用X射线衍射仪进行结构分析;
结论:碳量子点单一基质荧光膜为浅黄色薄膜,膜层厚度≤100nm,
产物纯度达99.8%;
(7)产物储存
将导电玻璃及其上的碳量子点单一基质荧光膜储存于棕色透明的玻璃容器内,密闭避光储存,要防晒、防潮、防酸碱盐侵蚀,储存温度20℃,相对湿度≤10%。
2.根据权利要求1所述的一种用碳量子点制备单一基质荧光膜的方法,其特征在于:制备碳量子点水溶液是在反应釜内进行的,是在配制溶液、加热炉加热、水热合成过程中完成的;
加热炉为立式,加热炉(1)的下部为炉座(2)、上部为炉盖(10),在加热炉(1)的内底部设有工作台(13),在工作台(13)上部置放反应釜(7),反应釜(7)上部为釜盖(11),在反应釜(7)内置放聚四氟乙烯容器(8),聚四氟乙烯容器(8)上部为容器盖(12),在聚四氟乙烯容器(8)内为混合溶液(9),并密闭;在炉座(2)上设有显示屏(3)、指示灯(4)、电源开关(5)、加热温度控制器(6)。
3.根据权利要求1所述的一种用碳量子点制备单一基质荧光膜的方法,其特征在于:用碳量子点单一基质荧光膜制备白光发光二极管:
①配制碳量子点单一基质荧光膜水溶液
将导电玻璃及其上的荧光膜置于烧杯中,滴入去离子水8mL,然后置于加热器上,加热温度30℃,加热时间40min,使碳量子点单一基质荧光膜溶解,成荧光膜溶液;
②打开发光二极管芯片座(14)上的透镜(21),将荧光膜溶液均匀滴入透镜(21)内,滴入量为0.03mL;
③将滴入荧光膜溶液的透镜置于真空干燥箱中干燥,干燥温度80℃,真空度6Pa,干燥时间180min;
④干燥后,将发光二极管芯片座(14)上的透镜(21)封盖,并密闭,即完成了白光发光二极管的制备。
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