CN105733556A - 一种量子点复合荧光颗粒、led模块 - Google Patents
一种量子点复合荧光颗粒、led模块 Download PDFInfo
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- CN105733556A CN105733556A CN201610161633.XA CN201610161633A CN105733556A CN 105733556 A CN105733556 A CN 105733556A CN 201610161633 A CN201610161633 A CN 201610161633A CN 105733556 A CN105733556 A CN 105733556A
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- quantum dot
- composite fluorescent
- dot composite
- module
- quantum
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Classifications
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- H01L33/502—Wavelength conversion materials
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C—CHEMISTRY; METALLURGY
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C—CHEMISTRY; METALLURGY
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
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- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
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- G02F1/133603—Direct backlight with LEDs
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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Abstract
本发明属于荧光材料领域,公开了一种量子点复合荧光颗粒,所述量子点复合荧光颗粒包括量子点、介孔材料和阻水阻氧材料,所述量子点分布在所述介孔材料中,在所述量子点和所述介孔材料之间的间隙填充有所述阻水阻氧材料。所述量子点复合荧光颗粒还包括金属纳米颗粒,所述金属纳米颗粒分布在所述介孔材料中。本发明还公开了应用该量子点复合荧光颗粒制成的LED模块。本发明在量子点和介孔材料之间的间隙填充阻水阻氧材料,大大提高了量子点复合荧光颗粒的水氧阻隔特性,因此提升了量子点复合荧光颗粒的稳定性;金属纳米颗粒可以帮助量子点俘获更多的蓝光,提高蓝光的利用率。
Description
技术领域
本发明属于荧光材料领域,涉及一种量子点复合荧光颗粒,还涉及应用该量子点复合荧光颗粒的LED模块。
背景技术
量子点是在把激子在三个空间方向上束缚住的半导体纳米结构,可以分成三类:胶质量子点,自组装量子点和电场约束量子点。量子点由于尺寸小于或接近于激子玻尔半径所引起的电子波函数的量子限制效应而产生许多独特的电学和光学性质,使其在生物化学、细胞生物学、免疫化学等学科的研究中显示出巨大的发展潜力,并已在激光器、单电子晶体管、探测器、生物染色、医疗诊断、DNA序列测定和免疫分析等方面得到应用。
量子点通常不能直接使用,因为量子点比较脆弱。自身由于纳米尺寸表面能较大,会发生团簇,造成荧光猝灭,容易发生能量转移;同时,胶质量子点的胶质层容易被侵蚀,留下缺陷能级,形成非辐射跃迁通道,造成荧光衰退。大部分的物理化学环境都会让量子点发生荧光猝灭。因此,如何使用量子点是目前一个比较热门和关键的一个问题。
在实际的应用过程中,通常的做法是直接将量子点分散到聚合物基体中得到荧光复合材料,形成简单“量子点-载体材料”的简单结构,复合材料基本上保持了胶体量子点的荧光特性,然后直接将复合材料结合蓝光LED得到白光,或者得到经过量子点转换的多色光谱,分别可以直接应用于显示和照明。
现有的使用量子点的方式主要有:直接通过搅拌的形式,将胶质量子点分散在硅胶中,然后将硅胶通过点胶的形式附着在LED上。该方法可以使用红绿量子点得到蓝/绿/红白光LED,也可以使用黄色量子点,如CuInS2系列的量子点,得到白光LED,同时也可以使用量子点配合荧光粉得到白光LED。然而该方法存在的问题是胶质量子点和硅胶的兼容性问题。由于量子点表面配体和硅胶载体材料不兼容,往往会出现量子点聚集,表面配体脱落引起的荧光猝灭;同时又由于水氧等因素,而硅胶对于水氧的阻隔差,在使用过程中,会由于水氧的侵蚀而引起量子点的荧光衰退,造成LED器件的寿命低下。同时,由于量子点表面(无机层和有机配体)中含有硫元素,会和现在商用的硅胶固话催化剂铂反应而使得硅胶不能固化。另一种方法是将量子点分散在聚合物材料中,得到量子点光转换薄膜,然后使用远离式的方式,将薄膜贴封在蓝光芯片上。该方法虽然改善了量子点和载体材料的兼容性问题,但聚合物对于水氧的阻隔仍然有限,在期间的长期工作中,仍然会面对量子点由于光致氧化带来的失效的问题。为了解决水氧等问题,采用二氧化硅/聚乙烯吡咯烷酮材料作为远离式封装的阻挡层,通过对复合薄膜作表面保护,在上下层加入阻水阻氧能力较好的薄膜,从而阻隔水和氧的侵入,减少对量子点表面的破坏。该方法虽然一定程度上能隔绝水氧,然而并不能阻止量子点的外表面和载体不兼容而造成的配体耗损和团聚效应,从而影响发光器件的稳定性和可靠性。同时,值得指出的是,对于这种远离式封装的LED而言,光效较之于芯片封装效果较差。
因此,要在器件中使用高发光效率和高稳定性的量子点,必须解决以下几个问题:1、量子点在自身表面处理或者和其他材料复合的时候,不能破坏其自身的发光效率;2、量子点的载体环境应该和量子点表面相兼容,一方面阻止量子点自身团聚,另一方面防止配体的脱落;3、设置阻挡层,阻止小分子如水汽和氧气对量子点表面的侵蚀。
发明专利201510576368.7公开了一种荧光量子点微纳米级封装的复合材料结构,复合材料结构包括荧光量子点、具有纳米栅格结构的介孔材料和阻挡层,其中荧光量子点分布在介孔材料中,阻挡层包覆在介孔材料的外表面。该阻挡层虽然可以很好的阻隔水氧,但是介孔材料中依然会残留水氧;并且阻挡层的包覆效果远远低于理论预期,对于水氧的阻隔效果并不理想。因此,需要对现有技术进行改进,获得阻水阻氧效果更好、效率更高的量子点复合材料。
发明内容
本发明的目的是提供一种阻水阻氧效果良好的量子点复合荧光颗粒。
本发明的另一目的是提供一种以该量子点复合荧光颗粒为光转换材料的LED器件。
为达到上述目的之一,本发明采用以下技术方案:
一种量子点复合荧光颗粒,所述量子点复合荧光颗粒包括量子点、介孔材料和阻水阻氧材料,所述量子点分布在所述介孔材料中,在所述量子点和所述介孔材料之间的间隙填充有所述阻水阻氧材料。
进一步地,所述量子点复合荧光颗粒还包括金属纳米颗粒,所述金属纳米颗粒分布在所述介孔材料中。
进一步地,所述金属纳米颗粒为纳米金、纳米银或纳米铂。
可以将金属纳米颗粒换成氧化物、半导体材料,同样可以和量子点形成LSPR效应。氧化物如氧化钨、氧化钒,半导体材料如二硫化钼、二硒化钼。
进一步地,所述金属纳米颗粒为圆形、三角形、方形或星形。其可以是任意形状,表面结构越粗糙,即棱角越多,表面增强的效果越明显。
进一步地,所述阻水阻氧材料为高分子聚合物。
进一步地,所述高分子聚合物为氧化聚乙烯蜡、聚乙烯、聚苯乙烯、聚对二甲苯、聚碳酸酯和聚甲基丙烯酸甲酯中的至少一种。
进一步地,所述介孔材料的粒径为0.05~1000μm;所述介孔材料的介孔孔径为2~50nm。
进一步地,所述介孔材料为介孔二氧化硅材料、介孔二氧化钛材料、介孔二氧化锌材料、分子筛或金属有机骨架化合物。
进一步地,所述量子点复合荧光颗粒还包括阻挡层,所述阻挡层包覆在所述介孔材料的外表面。
进一步地,所述阻挡层为氧化物介质层或聚合物介质层。
进一步地,所述氧化物为二氧化硅、二氧化钛或氧化硼;所述聚合物为聚苯乙烯或聚酰亚胺。
量子点是一种尺寸在2~50nm的晶体材料,一般由核心发光纳米晶体及其外延的无机壳层晶体,和最外延的有机配体层构成。
核心发光纳米晶体选自元素周期表中第II主族与第VI主族中的元素形成的第一化合物中的任意一种、第III主族与第V主族中的元素形成的第二化合物中的任意一种、所述第一化合物和/或所述第二化合物中的多种。所述第一化合物包括:CdSe、CdTe、MgS、MgSe、MgTe、CaS、CaSe、CaTe、SrS、SrSe、SrTe、BaS、BaSe、BaTe、ZnS、ZnSe、ZnTe和CdS;所述第二化合物包括:GaN、GaP、GaAs、InN、InP和InAs。
核心发光纳米晶体也可以选自CdSeS、CdZnSe、ZnSeS、CuInS2、CuInSe2、AgInS2、CdPbX3(X=Cl、Br、I)等。
外延的无机壳层晶体可以是CdS、ZnS、ZnSe、CdS/ZnS、CdS/ZnSe、CdZnSe、CdZnS等。
有机配体可以是油酸、硬脂酸、十六胺、十八胺、三辛基氧化磷等。
可以通过真空煅烧的方式、化学表面处理的方式实现介孔颗粒材料内表面的表面修饰,包括消除羟基、其他活性基团等,以实现荧光量子点和介孔颗粒材料的兼容性和荧光稳定性。
介孔材料的介孔孔径与量子点粒径匹配,使量子点能够嵌入到介孔材料的孔径中。
量子点分布嵌入介孔材料可以采用以下三种方法,但不限于以下方法:
1、使用物理法将量子点通过物理肿胀和溶剂挥发的方式嵌入介孔材料;
2、原位生长量子点,即在介孔材料中原位生长量子点;
3、原位生长介孔材料,即在量子点溶液中原位生长介孔材料。
一种LED模块,包括芯片、硅胶和量子点复合荧光颗粒,所述量子点复合荧光颗粒为前面所述的量子点复合荧光颗粒。
显示用白光LED的制备方法:将发红光的量子点复合荧光颗粒和发绿光的量子点复合荧光颗粒与硅胶混合,再通过搅拌、脱泡和点胶等工艺涂覆于蓝光芯片,得到白光LED。蓝光芯片发射的蓝光复合绿色荧光颗粒发射的绿光、红色荧光颗粒发射的红光得到蓝/绿/红三色白光LED。
将LED模块通过贴片等工艺得到白光灯条,然后集成到背光模组中,得到显示模组。显示模组有背光式和测光式两种:
一种LED背光式显示模组,包括液晶模组、匀光模组和背光模组,所述背光模组中集成有前面所述的LED模块。
一种LED侧光式显示模组,包括液晶模组、偏光模组、匀光模组、导光模组、背光模组和反光层,所述背光模组中集成有前面所述的LED模块。
照明用白光LED有两种,一种是用于照明的贴片式LED模块,包括蓝光芯片、黄色荧光粉、发红光的量子点复合荧光颗粒、硅胶、基板;另一种是用于照明的大功率LED模块,包括蓝光芯片、黄色荧光粉、发红光的量子点复合荧光颗粒、硅胶、基板、金线、PC透镜、引脚等。
照明用白光LED的制备方法:将发红光的量子点复合荧光颗粒和通用的黄色荧光粉与硅胶混合,再通过搅拌、脱泡和点胶等工艺涂覆于蓝光芯片,得到白光LED。蓝光芯片发射的蓝光复合荧光粉的黄光、红色荧光颗粒发射的红光,得到有红色光优化的白光,可以大大提高照明用白光的品质,尤其是显色指数。
本发明具有以下有益效果:
1、本发明在量子点和介孔材料之间的间隙填充阻水阻氧材料,可以使得量子点的载体材料更加致密,大大提高了量子点复合荧光颗粒的水氧阻隔特性,因此提升了量子点复合荧光颗粒的稳定性。
2、金属纳米颗粒可以帮助量子点俘获更多的蓝光,提高蓝光的利用率。在实际生产中,获得同样的光转换效果,可以减少量子点的使用,从而降低量子点中重金属的使用,更加绿色环保。
金属纳米颗粒对提高量子点荧光强度有两种作用机理:(1)纳米金属颗粒的自由电子在外界电磁场作用下规则运动而产生的表面等离子体可极大地增强粒子周围的电磁场,当入射光频率与金属颗粒自由电子固有频率一致时,产生表面等离子体共振,使局域场增强达到最大,这一增强的局域场使金属颗粒表面附近的量子点的激发速率得到增强,发光强度增强;(2)金属纳米颗粒与量子点的耦合辐射过程,量子点与金属颗粒之间发生非辐射能量转移,由激发的量子点耦合为LSPR能量,LSPR反过来辐射到远场。
3、本发明在制备过程中没有化学加工和化学处理,保存了量子点的荧光特性,包括发射波长和荧光效率,所得量子点复合荧光颗粒具有很高的量子效率。
4、量子点复合荧光颗粒具有介孔结构,从而大大减小了量子点在荧光颗粒中的聚集带来的效率衰退或者猝灭;量子点复合荧光颗粒具有阻挡层结构,减少了甚至完全阻隔了量子点和水氧的接触,提高了使用效率,使得量子点复合荧光颗粒及其LED模块具有优异的使用寿命,可直接用于商业化。
5、量子点复合荧光颗粒和LED芯片可以直接进行芯片接触式封装,大大提高了LED的光效。
6、量子点复合荧光颗粒直接调配得到显示用蓝/绿/红白光LED,也可以配合荧光粉得到照明用白光LED。
附图说明
图1是实施例1的量子点复合荧光颗粒的结构示意图;
图2是实施例1的量子点复合荧光颗粒随LED点亮时间的衰退示意图;
图3是实施例2的量子点复合荧光颗粒的荧光强度曲线;
图4是实施例3的量子点复合荧光颗粒的结构示意图;
图5是实施例4的贴片式LED的结构示意图;
图6是实施例4的LED背光式模组的结构示意图;
图7是实施例5的LED侧光式模组的结构示意图;
图8是实施例6的贴片式LED的结构示意图。
具体实施方式
下面结合具体实施例对本发明做进一步的说明:
以下实施例所用原料的质量配比、溶剂种类和用量、反应的温度和时间等条件,均可以按照实际需要灵活调整,属于本领域的常规技术手段。
实施例1
量子点复合荧光颗粒的制备:物理肿胀-溶剂挥发法。
1、介孔材料为介孔二氧化硅,粒径为30~60μm,介孔孔径为7~8nm,取1g介孔二氧化硅材料分散在100mL正己烷中,浸泡和活化介孔二氧化硅表面,然后加热回流,保温10h,加惰性气氛保护;
2、量子点为CdSe,平均尺寸为4~6nm,取10mg量子点分散到10mL正己烷中,再将量子点溶液分散到介孔二氧化硅溶液,快速搅拌2h,让量子点能够进入介孔二氧化硅;然后撤掉回流设备,鼓入惰性气氛,使得溶液几乎完全挥发,再加入新的溶液,通过不断改变浓度的方式,介孔二氧化硅在加热溶液中肿胀,使得量子点由于浓度差、有效率的进入介孔二氧化硅,反复肿胀-溶剂挥发操作,时间为1~10h;正己烷彻底挥发后,在惰性气体保护下,自然冷却,然后在真空干燥箱中干燥,得到量子点-介孔材料粉末;
3、取200mg氧化聚乙烯蜡分散至50mL甲苯,加热至固体融化,得到澄清透明的溶液;
4、将步骤2的量子点-介孔材料粉末加入到氧化聚乙烯蜡溶液中,快速搅拌,氧化聚乙烯蜡由于浓度差会进入介孔材料,填充量子点和介孔材料之间的间隙,待溶剂蒸发完全,得到量子点复合荧光颗粒。其结构如图1所示,1是量子点,2是介孔材料(介孔二氧化硅),3是阻水阻氧材料(氧化聚乙烯蜡)。
另外按照步骤1、2制备没有填充阻水阻氧材料的量子点复合荧光颗粒作为对比产品。
将对比产品和实施例产品制成LED,随着点亮时间增加,荧光颗粒的光转换效率衰退比率如图2所示,OPE(氧化聚乙烯蜡)填充的荧光颗粒(实心圆点)在一个月内光转换效率基本没有衰退,没有填充OPE的荧光颗粒(空心圆点)光转换效率逐步消退,一个月后剩余60%左右,这证明在量子点和介孔材料之间的间隙填充阻水阻氧材料后,提高了量子点复合荧光颗粒的水氧阻隔特性,进而提升其稳定性。
实施例2
含金属纳米颗粒的量子点复合荧光颗粒的制备:
1、取1g介孔二氧化硅和1mL三角形纳米金颗粒分散在100mL正己烷中,浸泡和活化介孔二氧化硅表面,然后加热回流,保温10h,加惰性气氛保护,撤掉回流系统,让溶剂蒸发,得到白色的金属-介孔二氧化硅复合颗粒粉末;
2、将得到的复合颗粒粉末在200℃、惰性气氛保护下煅烧处理,然后重新分散到50mL甲苯中;
3、取10mg发射波长在530nm的CdSe/ZnS量子点分散到10mL甲苯,再将量子点溶液分散到步骤2的金属-介孔二氧化硅溶液,快速搅拌2h,让量子点能够进入介孔二氧化硅;然后撤掉回流设备,鼓入惰性气氛,使得溶液几乎完全挥发,再加入新的溶液,通过不断改变浓度的方式,介孔二氧化硅在加热溶液中肿胀,使得量子点由于浓度差、有效率的进入介孔二氧化硅,反复肿胀-溶剂挥发操作,时间为1~10h;正己烷彻底挥发后,在惰性气体保护下,自然冷却,然后在真空干燥箱中干燥,得到量子点-介孔材料粉末;
4、取100mg聚乙烯分散至50mL氯仿,加热至固体融化,得到澄清透明的溶液;
5、将步骤3的量子点-介孔材料粉末加入到聚乙烯溶液中,快速搅拌,聚乙烯由于浓度差会进入介孔材料,填充量子点和介孔材料之间的间隙,待溶剂蒸发完全,得到含纳米金的绿色量子点复合荧光颗粒。
另外参照以上步骤制备没有加入纳米金的荧光颗粒。
当纳米金的吸收波长和量子点的发射波长匹配,且纳米金和量子点的间距合适时,金属颗粒可以通过等离子共振的方式参与发光,如图3所示,所得荧光颗粒的荧光强度(曲线1)比没有加入纳米金的荧光颗粒(曲线2)要强1.7倍。
实施例3
含金属纳米颗粒和阻挡层的量子点复合荧光颗粒的制备:
采用发射波长在640nm的CdSe/ZnS量子点,按照实施例2的步骤1~5进行,得到含纳米金的红色量子点复合荧光颗粒。
然后将其重新分散到无水酒精中,添加纯度为99.99%的正硅酸乙酯,均匀搅拌,逐滴加入氨水,加速搅拌,水解正硅酸乙酯,生长二氧化硅介质层。得到含金属纳米颗粒和阻挡层的量子点复合荧光颗粒。其结构如图4所示,1是量子点,2是介孔材料(介孔二氧化硅),3是金属纳米颗粒(纳米金),4是阻水阻氧材料(聚乙烯),5是阻挡层(二氧化硅介质层)。
实施例4
用于显示的LED背光式模组
如图5所示,将50mg发红光的量子点复合荧光颗粒1、50mg发绿光的量子点复合荧光颗粒2与1g硅胶3混合,快速、均匀搅拌硅胶混合物,真空脱泡,然后将混合物通过点胶涂覆于蓝光芯片4,得到白光LED(5)。
如图6所示,LED(1)通过贴片等工艺得到白光灯条,然后集成到背光模组2中,背光模组2和液晶模组3、匀光模组4构成LED背光式模组。
蓝光芯片发射的蓝光复合绿色荧光颗粒发射的绿光、红色荧光颗粒发射的红光得到蓝/绿/红三色白光LED。
实施例5
用于显示的LED侧光式模组
将50mg发红光的量子点复合荧光颗粒、50mg发绿光的量子点复合荧光颗粒与1g硅胶混合,快速、均匀搅拌硅胶混合物,真空脱泡,然后将混合物通过点胶涂覆于蓝光芯片,得到白光LED。
如图7所示,LED(1)通过贴片等工艺得到白光灯条,然后集成到背光模组2中,背光模组2和液晶模组3、偏光模组4、匀光模组5、导光模组6、反光层7构成LED侧光式模组。
蓝光芯片发射的蓝光复合绿色荧光颗粒发射的绿光、红色荧光颗粒发射的红光得到蓝/绿/红三色白光LED。
实施例6
用于照明的贴片式LED模块
1、如图8所示,取50mg发红光的量子点复合荧光颗粒1和10mg黄色荧光粉2,与1g硅胶3混合。
2、快速、均匀搅拌硅胶混合物,真空脱泡,然后将混合物通过点胶的形式点在含蓝光芯片4的贴片式LED上。
3、在100~150℃固化,得到白光LED(5)。
蓝光芯片发射的蓝光复合荧光粉的黄光、红色荧光颗粒发射的红光,得到有红色光优化的白光,显色指数得到提升。该白光LED显色指数R8在95以上,R9在95以上,光效在20mA电流下达到120lm/W以上。
实施例7
用于照明的大功率LED模块
1、取50mg发红光的量子点复合荧光颗粒和10mg黄色荧光粉,与1g硅胶混合。
2、快速、均匀搅拌硅胶混合物,真空脱泡,然后将混合物通过点胶的形式点在含蓝光芯片的贴片式(大功率式)LED上。
3、在100~150℃进行固化,得到白光LED。
4、安装引脚和金线,盖上聚碳酸酯透镜,注入填充硅胶,再次在100~150℃下固化,得到大功率型高光效高显色指数的白光LED。
蓝光芯片发射的蓝光复合荧光粉的黄光、红色荧光颗粒发射的红光,得到有红色光优化的白光,显色指数得到提升。该大功率白光LED的显色指数R8在95以上,R9在95以上,光效在20mA电流下达到150lm/W以上。
实施例8
1、介孔材料为介孔二氧化硅,粒径为30~60μm,介孔孔径为7~8nm,取500mg介孔二氧化硅材料分散在100mL甲苯;
2、量子点为ZnSeS,取10mg量子点分散到10mL甲苯,再将量子点溶液加入介孔二氧化硅溶液,在100℃回流1h,快速搅拌;撤走回流设备,让甲苯蒸发完全,得到量子点-介孔材料粉末;
3、将上述粉末放入真空腔,并缓慢通入派瑞林单体(对二甲苯)气体源,让单体沿着量子点和介孔材料之间的间隙聚合填充,得到量子点复合荧光颗粒。
实施例9
1、介孔材料为介孔二氧化钛,粒径为0.05~10μm,介孔孔径为2~10nm,取200mg介孔二氧化钛材料分散在30mL正己烷;
2、量子点为SrTe,取4mg量子点分散到5mL正己烷,再将量子点溶液加入介孔二氧化钛溶液,加热回流,然后撤掉回流设备,让溶剂蒸发完全,量子点进入介孔二氧化钛,得到量子点-介孔材料粉末;
3、取40mg聚苯乙烯分散至20mL正己烷,加热至固体融化,得到澄清透明的溶液;
4、将步骤2的量子点-介孔材料粉末加入到聚苯乙烯溶液中,快速搅拌,聚苯乙烯由于浓度差会进入介孔材料,填充量子点和介孔材料之间的间隙,待溶剂蒸发完全,得到量子点复合荧光颗粒。
5、在量子点复合荧光颗粒表面生长二氧化钛介质层作为阻挡层。
实施例10
1、取2g介孔二氧化锌(粒径为100~1000μm,介孔孔径为10~50nm)和2mL星形纳米银颗粒分散在300mL甲苯,浸泡和活化介孔二氧化锌表面,然后加热回流,保温10h,加惰性气氛保护,撤掉回流系统,让溶剂蒸发,得到金属-介孔二氧化锌复合颗粒粉末;
2、将得到的复合颗粒粉末在200℃、惰性气氛保护下煅烧处理,然后重新分散到200mL甲苯;
3、取50mgInP量子点分散到20mL甲苯,再将量子点溶液加入步骤2的金属-介孔二氧化锌溶液,加热回流,然后撤掉回流设备,让溶剂蒸发完全,量子点进入介孔二氧化锌,得到量子点-介孔材料粉末;
4、取400mg聚碳酸酯分散至150mL甲苯,加热至固体融化,得到澄清透明的溶液;
5、将步骤3的量子点-介孔材料粉末加入到聚碳酸酯溶液中,快速搅拌,聚碳酸酯由于浓度差会进入介孔材料,填充量子点和介孔材料之间的间隙,待溶剂蒸发完全,得到含纳米银的量子点复合荧光颗粒。
实施例11
1、取1g分子筛和0.5mL圆形纳米铂颗粒分散在100mL氯仿,浸泡和活化分子筛表面,然后加热回流,保温10h,加惰性气氛保护,撤掉回流系统,让溶剂蒸发,得到金属-分子筛复合颗粒粉末;
2、将得到的复合颗粒粉末在200℃、惰性气氛保护下煅烧处理,然后重新分散到40mL氯仿;
3、取20mgCuInSe2量子点分散到10mL氯仿,再将量子点溶液加入步骤2的金属-分子筛溶液,加热回流,然后撤掉回流设备,让溶剂蒸发完全,量子点进入分子筛,得到量子点-介孔材料粉末;
4、取200mg聚甲基丙烯酸甲酯分散至100mL氯仿,加热至固体融化,得到澄清透明的溶液;
5、将步骤3的量子点-介孔材料粉末加入到聚甲基丙烯酸甲酯溶液中,快速搅拌,聚甲基丙烯酸甲酯由于浓度差会进入介孔材料,填充量子点和介孔材料之间的间隙,待溶剂蒸发完全,得到含纳米铂的量子点复合荧光颗粒。
6、在量子点复合荧光颗粒表面生长氧化硼介质层作为阻挡层。
实施例12
1、取1.5g介孔二氧化硅和0.5g二硫化钼粉末分散在100mL正己烷,浸泡和活化介孔二氧化硅表面,然后加热回流,保温10h,加惰性气氛保护,撤掉回流系统,让溶剂蒸发,得到半导体-介孔二氧化硅复合颗粒粉末;
2、将得到的复合颗粒粉末在200℃、惰性气氛保护下煅烧处理,然后重新分散到80mL正己烷;
3、取10mgCdS/ZnSe量子点分散到10mL正己烷,再将量子点溶液加入步骤2的半导体-介孔二氧化硅溶液,加热回流,然后撤掉回流设备,让溶剂蒸发完全,量子点进入介孔二氧化硅,得到量子点-介孔材料粉末;
4、取80mg氧化聚乙烯蜡分散至100mL正己烷,加热至固体融化,得到澄清透明的溶液;
5、将步骤3的量子点-介孔材料粉末加入到氧化聚乙烯蜡溶液中,快速搅拌,氧化聚乙烯蜡由于浓度差会进入介孔材料,填充量子点和介孔材料之间的间隙,待溶剂蒸发完全,得到含二硫化钼的量子点复合荧光颗粒。
6、在量子点复合荧光颗粒表面包覆聚苯乙烯作为阻挡层。
除上述方法外,阻水阻氧材料的填充方式,还可以采用原位聚合法:聚合物单体和引发剂进入量子点-介孔材料,原位反应填充间隙。
以上所述,仅为本发明的具体实施方式,但本发明的保护范围并不局限于此,任何属于本技术领域的技术人员在本发明揭露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求的保护范围为准。
Claims (14)
1.一种量子点复合荧光颗粒,其特征在于,所述量子点复合荧光颗粒包括量子点、介孔材料和阻水阻氧材料,所述量子点分布在所述介孔材料中,在所述量子点和所述介孔材料之间的间隙填充有所述阻水阻氧材料。
2.根据权利要求1所述的量子点复合荧光颗粒,其特征在于,所述量子点复合荧光颗粒还包括金属纳米颗粒,所述金属纳米颗粒分布在所述介孔材料中。
3.根据权利要求2所述的量子点复合荧光颗粒,其特征在于,所述金属纳米颗粒为纳米金、纳米银或纳米铂。
4.根据权利要求2所述的量子点复合荧光颗粒,其特征在于,所述金属纳米颗粒为圆形、三角形、方形或星形。
5.根据权利要求1或2所述的量子点复合荧光颗粒,其特征在于,所述阻水阻氧材料为高分子聚合物。
6.根据权利要求5所述的量子点复合荧光颗粒,其特征在于,所述高分子聚合物为氧化聚乙烯蜡、聚乙烯、聚苯乙烯、聚对二甲苯、聚碳酸酯和聚甲基丙烯酸甲酯中的至少一种。
7.根据权利要求1或2所述的量子点复合荧光颗粒,其特征在于,所述介孔材料的粒径为0.05~1000μm;所述介孔材料的介孔孔径为2~50nm。
8.根据权利要求1或2所述的量子点复合荧光颗粒,其特征在于,所述介孔材料为介孔二氧化硅材料、介孔二氧化钛材料、介孔二氧化锌材料、分子筛或金属有机骨架化合物。
9.根据权利要求1或2所述的量子点复合荧光颗粒,其特征在于,所述量子点复合荧光颗粒还包括阻挡层,所述阻挡层包覆在所述介孔材料的外表面。
10.根据权利要求9所述的量子点复合荧光颗粒,其特征在于,所述阻挡层为氧化物介质层或聚合物介质层。
11.根据权利要求10所述的量子点复合荧光颗粒,其特征在于,所述氧化物为二氧化硅、二氧化钛或氧化硼;所述聚合物为聚苯乙烯或聚酰亚胺。
12.一种LED模块,其特征在于,包括芯片、硅胶和量子点复合荧光颗粒,所述量子点复合荧光颗粒为权利要求1或2所述的量子点复合荧光颗粒。
13.一种LED背光式显示模组,包括液晶模组、匀光模组和背光模组,其特征在于,所述背光模组中集成有权利要求12所述的LED模块。
14.一种LED侧光式显示模组,包括液晶模组、偏光模组、匀光模组、导光模组、背光模组和反光层,其特征在于,所述背光模组中集成有权利要求12所述的LED模块。
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