CN110396107B - 一种高稳定黄色发光手性纳米银簇材料及其在白光led中的应用 - Google Patents
一种高稳定黄色发光手性纳米银簇材料及其在白光led中的应用 Download PDFInfo
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Abstract
本发明公开了一种高稳定黄色发光手性纳米银簇材料及其在白光LED中的应用，属于纳米材料和配位化学的交叉领域。所述手性纳米银簇以手性配体(R)‑4‑异丙基噻唑烷‑2‑硫酮（D）为保护配体，通过简单的室温挥发一锅法合成产量高，纯黄色发光性能优越的手性银纳米团簇。该纳米银簇的化学式为:C36H60Ag6N6S12(简写为：Ag6D6)，属于立方晶系，空间群为手性空间群P21。该团簇在室温下具有较强的纯黄色荧光，荧光量子产率为56%；其结构可以稳定到160℃，并且仍然保持发光；其手性结构以及强烈的发光性质赋予该团簇结构较强的圆偏振发光（CPL）性质。该银纳米团簇稳定性高，蓝色波段可激发出强的纯黄色荧光使其可以作为白光LED的黄光荧光粉。
Description
技术领域
本发明属于纳米材料和配位化学的交叉领域，具体涉及一种高稳定黄色发光手性纳米银簇材料及其在白光LED中的应用。
背景技术
原子精确的纳米银簇是外层由有机配体保护，内核由3个或3个以上金属银原子通过亲银作用所形成的尺寸在1–3nm之间的一类具有精确原子结构的簇合物。纳米团簇是介于原子、分子与体相材料之间的一种物质状态，是连接原子、分子与宏观物质的桥梁，其尺寸一般是纳米量级，往往会伴随有量子限域效应而产生许多新的现象和性质。其优异的光物理性能及其在催化、生物成像等领域的潜在应用而成为近年来材料和无机化学的研究热点。
目前对纳米银簇的研究主要集中于新型纳米团簇的合成与应用方面。目前报道的银纳米团簇室温条件下的稳定性都比较差，而且发光效率都比较低，这些缺陷就大大阻碍了纳米团簇的应用和发展，所以设计合成原子精确、结构稳定、发光效率高的银纳米团簇是纳米团簇领域研究重点之一。
LED即是发光二极管，是一种半导体固体发光器件，因其节能、环保、寿命长、体积小等优点而成为现代一种新型的照明产品。白光LED因其本身的诸多优势正逐渐取代现有的照明灯而成为主流的照明产品。目前市场上白光LED生产技术主要通过两种方法形成：第一种是多种单色光混合法，使用多种可以发出不同单色光的荧光粉材料通过紫外光激发产生的单色光混合形成白光，该方法产生白光方式复杂，存在高耗能、紫外线泄露等缺点；第二种是使用通过蓝光芯片搭配黄光荧光粉，通过蓝光激发黄光荧光粉产生单一纯色黄光与蓝光组合而形成白光，该方法简单安全低能耗，是最普遍生产白光LED的方法。所以稳定性高，蓝光可激发纯色单一黄色发光的纳米银簇在白光LED方面具有很好的应用前景。
发明内容
本发明目的在于提供高稳定黄色发光手性纳米银簇材料及其在白光LED中的应用。
为实现本发明的目的，本发明研发了一种高稳定黄色发光手性纳米银簇材料，所述纳米银簇的化学式是：C36H60Ag6N6S12(简写为：Ag6D6)，属于立方晶系；空间群为手性空间群P21，
其中D为(R)-4-异丙基噻唑烷-2-硫酮，结构简式如下：
本发明纳米银簇的制备方法通过如下步骤实现：
将配体(R)-4-异丙基噻唑烷-2-硫酮溶解于N,N-二甲基乙酰胺(DMAc)和乙腈混合溶液中，室温搅拌溶解澄清；加入硝酸银，搅拌溶解澄清，再室温搅拌反应5分钟，反应结束以后将澄清溶液置于室温下避光挥发，得晶体，过滤，用乙腈洗涤，室温晾干即可。
所述纳米银簇是一个由六个银原子组成的内核，外围由六个有机配体保护(图1所示)。六个银原子通过亲银相互作用形成一个扭曲的八面体内核(图2所示)，六个有机配体分别分布于八面体的六个面上，每个配体上的巯基硫原子与两个银原子配位，每个氮原子连接一个银原子(图3所示)。
本发明纳米银簇材料用于白光LED的应用，其性质具体描述如下：
所述材料具有超稳定的晶体结构，在160℃高温下仍然可以保持晶态结构和发光(图4和5所示)。在空气室温条件下具有强烈的亮黄色荧光，其最佳发射波长位置为556nm(激发波长370nm)(图6所示)；室温条件下的荧光寿命为16μs；室温条件下荧光量子产率为56％。该材料可以被蓝光波段激发出强烈的纯黄色荧光(图7所示)；将该材料的固体粉末均匀涂抹在蓝光LED灯泡的表面，点亮LED灯，蓝光将该材料激发出纯黄色荧光，黄色荧光与蓝光组合在一起形成白光(图8所示)。
本发明有益效果：本发明纳米银簇材料具有很宽的激发波段，可以被蓝光激发出强的纯黄色荧光；另外所述纳米银簇材料具有很高的稳定性，可以稳定到160℃仍然保持晶态结构，在白光LED方面具有很好的应用价值。
附图说明
图1为本发明纳米银簇材料单晶结构示意图。
图2为本发明纳米银簇材料的内核结构示意图。
图3为本发明纳米银簇材料的配体配位模式示意图。
图4为本发明纳米银簇材料变温(30℃到150℃)XRD图。
图5为本发明纳米银簇材料在不同温度下的粉末晶体荧光照片(365nm紫外灯下)，图中第一张为日光灯照片，其余是不同温度下的荧光照片。
图6为本发明纳米银簇材料激发曲线和发射曲线图。
图7为本发明纳米银簇材料不同激发波长下的发射曲线(300nm-480nm)。
图8为本发明纳米银簇材料作为黄光荧光粉与蓝光LED灯组装成的白光LED灯，图中1是使用的蓝光LED灯，2是涂抹纳米银簇材料粉末的LED灯，3是点亮以后发白光的LED(其中插图是测试的该白光LED发出的白光曲线图)。
具体实施方式
下面通过实例对本发明做进一步的说明：
实施例1：本发明纳米银簇材料的合成
将16mg(0.1mmol)(R)-4-异丙基噻唑烷-2-硫酮(D)溶解于3mL DMAc和1mL乙腈的混合溶液中，快速搅拌；加入19mg(0.1mmol)AgNO3搅拌至溶液澄清，再室温搅拌反应5分钟，反应结束以后将澄清溶液置于室温下避光挥发，2天以后得浅黄色块状晶体，产率74％，过滤，用乙腈洗涤，室温晾干用于其性质测试材料。
实施例2：本发明纳米银簇材料作为黄光荧光粉组装白光LED
取实施例1制得的本发明纳米银簇材料样品，研磨成细小的固体粉末，加入到乙酸乙酯里面超声均匀，将分散溶液滴加到蓝光LED灯泡表面，溶剂挥发干以后形成一层均匀的固体粉末膜。
取实施例1制得的本发明纳米银簇材料做进一步表征，其过程如下：
(1)晶体结构测定
配合物的X射线单晶衍射数据用大小合适的单晶样品在Rigaku XtaLAB Pro单晶衍射仪上测定。数据均用经石墨单色化的CuKα射线
为衍射源通过ω扫描方式在150K温度下收集，并经过Lp因子校正和半经验吸收校正。结构解析是先通过SHELXS-97程序用直接法得到初结构，然后使用SHELXL-97程序用全矩阵最小二乘法精修。所有非氢原子均采用各向异性热参数法精修。所有的氢原子都采用各向同性热参数法精修。详细的晶体测定数据见表1；重要的键长数据见表2。
表1本发明纳米银簇材料的主要晶体学数据
表1主要晶体学数据
R1＝∑||Fo|-|Fc||/∑|Fo|.wR2＝[∑w(Fo 2-Fc 2)2/∑w(Fo 2)2]1/2
表2 Ag6D6重要的键长
| Ag1-Ag1<sup>1</sup> | 3.3275(15) | Ag1-Ag1<sup>2</sup> | 3.3275(15) |
| Ag1-Ag2<sup>2</sup> | 3.2373(13) | Ag1-Ag2 | 2.9627(13) |
| Ag2-Ag1<sup>1</sup> | 3.3273(13) | Ag2-Ag2<sup>2</sup> | 3.3478(17) |
| Ag2-Ag2<sup>1</sup> | 3.3478(17) | Ag1-S1<sup>2</sup> | 2.523(3) |
| Ag1-S1 | 2.451(3) | Ag1-N1 | 2.237(12) |
| Ag2-S2 | 2.433(5) | Ag2-S2<sup>1</sup> | 2.496(5) |
| Ag2-N2 | 2.275(10) | S2-Ag2<sup>2</sup> | 2.496(5) |
| S1-Ag1<sup>1</sup> | 2.523(3) |
对称代码:11/2-z,1-x,-1/2+y；21-y,1/2+z,1/2-x.
以上实施例仅用于说明本发明的内容，除此之外，本发明还有其它实施方式。但是，凡采用等同替换或等效变形方式形成的技术方案均落在本发明的保护范围内。
Claims (1)
1.一种手性纳米银簇材料在发光材料方面的应用，其特征在于：将该材料的固体粉末均匀涂抹在蓝光LED灯泡的表面，点亮LED灯，蓝光将该材料激发出纯黄色荧光，黄色荧光与蓝光组合在一起形成白光；
该手性纳米银簇材料化学式是：C36H60Ag6N6S12 ，简写为：Ag6D6，属于立方晶系；空间群为手性空间群P21，a , b，c = 18.10900(10) Å, V = 5938.59(10) Å3；
其中D为(R)-4-异丙基噻唑烷-2-硫酮，结构简式如下：
该手性纳米银簇材料是由六个银原子组成的内核，外围由六个有机配体保护，六个银原子通过亲银相互作用形成一个扭曲的八面体内核，六个有机配体分别分布于八面体的六个面上，每个配体上的巯基硫原子与两个银原子配位，每个氮原子连接一个银原子；其单晶结构如附图1。
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