CN114736674B - 一种led用固态聚集不猝灭型白光碳点的制备方法 - Google Patents
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Abstract
本发明属于发光材料技术领域,具体涉及一种LED用固态聚集不猝灭型白光碳点的制备方法。所述方法包括以下步骤:(1)以柠檬酸为碳源,以硼酸和硅酸为掺杂剂,将上述原料溶于水中,混匀;(2)步骤(1)得到的混合物在200‑250℃进行热解,得到白光碳点。本发明制备方法工艺简单,适宜工业化,且制备成本低廉,过程环保;制得的白光碳点具有固态聚集态时发光稳定、不猝灭,并且其发光具有耐高温的特点;所制备的碳点可应用于白光LED,以及柔性显示和超薄显示方面。
Description
技术领域
本发明属于发光材料技术领域,具体涉及一种LED用固态聚集不猝灭型白光碳点的制备方法。
背景技术
目前,照明的能源消耗占全球能源消耗大约22%左右,高效节能的照明设备有可能减少一半的能源消耗,进而降低相应的碳排放,实现碳达峰的目标。LED作为第四代照明技术,因其能耗低、使用寿命长而日益受到业界的广泛关注。目前商用白光LED的制备主要有两种方式,即蓝光芯片与黄色荧光粉、紫外芯片与RGB(红、绿、蓝)三基色荧光粉。常用的荧光粉主要为昂贵的稀土荧光粉,其成本较高。寻找廉价、高效的新型LED用荧光粉也日益成为一个需要解决的问题。相对于稀土荧光粉,碳点具有低成本、环境友好等优点。
碳点是一种具有光致发光的碳基零维纳米材料,尺寸常常在10nm以下,因为碳点具有多色荧光性、生物相容性、优异的水溶性、低毒性等优良特性,而受到广泛关注。迄今,合成碳点的方法有多种:如水热法(CN202110695392.8)、溶剂热法、微波法、超声波法、等离子体法和激光烧蚀法等等。合成的碳点大多数因为其自身性质的原因,常常在液体中能表现优良的光致发光性能,而聚集成固体状态时常常表现为发光猝灭(Journal of Colloidand Interface Science,2021,598:274-282)。因此,将碳点作为荧光粉应用于LED,就必须要解决碳点材料在聚集态发生荧光猝灭的问题,进而制备出发光稳定的LED器件。而且,碳点发光也不耐高温,在自然环境中结构不稳定,长期放置容易发生结构变化而导致发光猝灭。
目前文献报道的大多数碳点LED器件都采用在碳点外包覆其他耐温材料或制成多种材料复合薄膜来实现碳点LED器件的制备(Carbon,2022,190:22-31)。而且,目前文献报道的白光碳点LED器件通常采用类似稀土三基色白光LED的制备工艺,即采用互补色碳点共混的工艺制备白光碳点LED器件,即将蓝色和黄色碳点、或者是红绿蓝三色碳点按照一定的质量比混合(Advanced Materials,2018,30(1):1704740.)来制备白光碳点LED器件;这一制备过程需要大量的实验尝试并进行相关的LED器件测试,最终才能确定碳点混合的最优比例,过程复杂且不利于工业化。另外,虽然有部分文献报道白光碳点可以直接合成,但是其合成步骤较为复杂,且合成条件较为苛刻,例如冷冻干燥法较为耗时,水热法的工业化放大需要昂贵的反应设备,器件制备成本相应增加。所以,寻找一种能够快速、高效的合成在固体聚集态时发光稳定、不猝灭的白光碳点的方法,是十分迫切的。
发明内容
本发明的目的是提供一种LED用固态聚集不猝灭型白光碳点的制备方法,采用一步热解法制备白光碳点,该碳点具有特殊的表面杂原子掺杂,在固态聚集时发光稳定,不发生荧光猝灭,且其发光性能具有耐高温的特性。
为了实现上述目的,本发明的技术方案如下:
本发明一方面提供一种LED用固态聚集不猝灭型白光碳点的制备方法,所述方法包括以下步骤:
(1)以柠檬酸为碳源,以硼酸和硅酸为掺杂剂,将上述原料溶于水中,混匀;
(2)步骤(1)得到的混合物在200-250℃进行热解,得到白光碳点。
上述技术方案中,进一步地,所述步骤(1)中柠檬酸、硼酸、硅酸、水的质量比为1:3:(0.01~1):50。
上述技术方案中,进一步地,所述步骤(2)中热解时间为4~6h。
上述技术方案中,进一步地,通过调控Si原子在碳点中的掺杂浓度,调控白光的色温。
本发明另一方面提供一种上述制备方法制得的白光碳点。
本发明再一方面提供一种上述碳点在制备白光LED器件上的应用,将碳点与370nm发射LED芯片进行封装,得到白光LED器件。
本发明制得的碳点有较好的发光稳定性和固态聚集时发光不猝灭的特点。通过调控Si原子在碳点中的掺杂浓度,可以调控白光的色温。
本发明的有益效果为:
本发明制备方法工艺简单,适宜工业化,且制备成本低廉,过程环保;制得的白光碳点具有固态聚集态时发光稳定、不猝灭,并且其发光具有耐高温的特点;所制备的碳点可应用于白光LED,以及柔性显示和超薄显示方面。
附图说明
图1为实施例1-5制得的白光碳点的发射光谱(激发波长为365nm);
图2为实施例3制得的白光碳点的变温发射光谱(激发波长为365nm);
图3为实施例3制得的白光碳点的发光强度值随温度变化图(激发波长为365nm);
图4为实施例3制得的白光碳点放置于自然环境下发光强度随时间变化图(激发波长为365nm);
图5为实施例3制得的白光碳点的XRD图;
图6为实施例3制得的白光碳点TEM图;
图7为实施例3制得的白光碳点傅里叶红外光谱图;
图8为实施例3制得的白光碳点LED实物图;
图9为实施例3制得的白光碳点的色坐标图。
具体实施方式
以下实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
实施例1
称量2g柠檬酸、6g硼酸、0.05g硅酸混合,完全溶解于100ml去离子水中,将此溶液置于230℃烘箱中热解反应5h,形成最终产物记为白光碳点-1。
实施例2
称量2g柠檬酸、6g硼酸、0.1g硅酸混合,完全溶解于100ml去离子水中,将此溶液置于230℃烘箱中热解反应5h。形成最终产物记为白光碳点2。
实施例3
称量2g柠檬酸、6g硼酸、0.2g硅酸混合,完全溶解于100ml去离子水中,将此溶液置于230℃烘箱中热解反应5h。形成最终产物记为白光碳点3。
实施例3制得的白光碳点3的色坐标如图9所示,色坐标为(0.32,0.36),色温为6275.99K,显色指数89。
实施例4
称量2g柠檬酸、6g硼酸、0.5g硅酸混合,完全溶解于100ml去离子水中,将此溶液置于230℃烘箱中热解反应5h。形成最终产物记为白光碳点4。
实施例5
称量2g柠檬酸、6g硼酸、1g硅酸混合,完全溶解于100ml去离子水中,将此溶液置于230℃烘箱中热解反应5h。形成最终产物记为白光碳点5。
实施例1-5制得的白光碳点的色温变化表如表1所示。
表1实施实例1-5制得的白光碳点的色温
样品 | 色温 |
实施例1 | 5459.388K |
实施例2 | 5996.111K |
实施例3 | 6275.990K |
实施例4 | 6076.116K |
实施例5 | 8016.448K |
实施例6
将实施例3制得的白光碳点3与市售的370nm发射LED芯片进行封装,得到白光LED器件:
用电子天平称量0.05g的碳点,并称量A胶0.25g和B胶1g。将称量好的A胶进行搅拌,搅拌时间为2min,然后向其中加入CDs,再搅拌混合至均匀。将称好的B胶加入上述的A胶和CDs的混合物中,再搅拌混合至均匀,搅拌时长为5min;然后用低频超声波进行脱泡。将脱泡后的混合物蘸取、并点胶于LED基底支架上,点胶好的LED放入烘箱中,在60℃下烘烤40min,然后在135℃下烘烤110min,得到封装后的白光LED器件。
白光碳点LED实物图如图8所示。
Claims (4)
1.一种固态聚集不猝灭型白光碳点的制备方法,其特征在于,所述方法包括以下步骤:
(1)以柠檬酸为碳源,以硼酸和硅酸为掺杂剂,将上述原料溶于水中,混匀,柠檬酸、硼酸、硅酸、水的质量比为1:3:(0.01-1):50;
(2)步骤(1)得到的混合物在200-250 ℃进行热解4-6 h,得到白光碳点。
2.根据权利要求1所述的制备方法,其特征在于,通过调控Si原子在碳点中的掺杂浓度,调控白光的色温。
3.一种权利要求1-2任一项所述制备方法制得的白光碳点。
4.一种权利要求3所述白光碳点的应用,其特征在于,将碳点与370 nm发射LED芯片进行封装,得到白光LED器件。
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