水溶性量子点和量子点/分子筛纳米复合材料的制备及其应用研究
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摘要
白光发光二极管(白光LED)由于其寿命长、环保、效率高等优点,将成为新一代固体照明光源。目前,商业白光LED主要是通过荧光转换法将Y3A15O12:Ce3+(YAG:Ce)黄色荧光粉涂于蓝光LED芯片上来实现,但是由于缺乏红色成分导致白光LED的显色指数不高,发光效率低等缺陷,所以寻求一种发光效率高、稳定性好的荧光材料成为白光LED研究中的一个热点。量子点作为一种新型的纳米材料,由于存在量子限域效应,使其表现出独特的荧光性能。相对于有机染料而言,量子点存在很多优点,如激发光谱宽、颜色可调、抗光漂白等。由于这些独特的性质,量子点在生物医学、光电器件以及催化等领域表现出很好的应用前景。目前,大多数商业用量子点都是通过传统的有机金属法合成,其合成过程毒性较大。本文从应用的要求出发,采用绿色环保的巯基水相法合成适用于LED用的量子点。对所合成的量子点的结构组成、形貌特征、光谱性能等进行了表征。将实验所合成的部分量子点应用于白光LED中,并对所组装白光LED的相关技术指标进行了详细地讨论。除此之外,还通过采用Y型分子筛作为主体材料,在Y型分子筛中合成规则有序的量子点,并对其光催化性能进行详细地研究。具体开展了以下工作：
(1)在水相体系中,通过一步水相法成功地合成了巯基乙胺(CA)稳定的CdTe量子点。CA-CdTe量子点为近球形的闪锌矿结构；通过控制体系的反应时间来调节CdTe量子点的发射波长,结果表明,随着回流时间的延长,其最大荧光发射波长发生明显的红移现象,表现出明显的量子尺寸效应。通过对反应温度、前驱体溶液的pH值、Cd与Te的物质的量比等条件的优化,得到了一个巯基乙胺稳定CdTe量子点水相合成的最优合成方案：n(Cd):n (Te2-):n(CA)=1:0.05:2,pH为5.85,温度为100℃,并且最大荧光量子产率可以达到10.73%。
(2)用巯基乙酸作为稳定剂,通过一锅水相法成功地合成了一系列不同Mn离子量掺杂的CdTe纳米粒子。XRD和HRTEM结果表明,样品具有闪锌矿结构CdTe量子点的特征峰,说明Mn离子的加入并没有改变CdTe量子点的晶体结构；并且样品为近球型形状,直径约为3nm。Mn离子的加入使得CdTe量子点的荧光发射光谱发生明显的红移现象,使得更加容易得到红光发射的量子点,可将其应用于商业白光LED以弥补商业荧光粉的缺陷。
(3)以Na2TeO3为碲源,分别以硫普罗宁(TP)、L-半胱氨酸(Cys)和巯基丁二酸(MSA)作为稳定剂,在水相体系中合成水溶性的CdTe量子点。XRD和HRTEM结果表明三种不同稳定剂稳定的CdTe量子点都呈球状的闪锌矿结构,且分散均匀。实验结果表明,分别用三种稳定剂稳定的CdTe量子点均在碱性条件下合成,并且稳定剂的种类对量子点在水相介质中的尺寸分布和生长率有很大的影响。从它们的荧光发射峰可以看出,MSA稳定的CdTe量子点的生长速度最快,当回流到7h时其最大荧光发射达到了650nm的红光发射。TP稳定的CdTe量子点的生长速度最慢,当回流7h时的最强发射波长只有586nm。
(4)分别以ZnCl2、CdCl2、TeO2为Zn源,Cd源和Te源,采用一锅水相法合成水溶性蓝光发射的ZnxCd(1-x)Te量子点。实验结果表明,通过改变Zn2+/Cd2+摩尔比可以调节合金化合物的发光颜色。随着Zn2+/Cd2+摩尔比的增加,ZnxCd(1-x)Te合金型量子点的发射波长发生明显的蓝移现象,当Zn2+/Cd2+摩尔比为70：2时,ZnxCd(1-x)Te合金型量子点发出460nm左右的蓝光。通过对实验合成的ZnCdTe量子点的表面进行修饰,在ZnCdTe量子点的外表面再生长一层CdSe量子点壳,生成黄光发射的ZnCdTe/CdSe核／壳型纳米晶体,可作为白光LED用黄色荧光粉。
(5)采用荧光转换法,用单核的巯基丙酸(MPA)稳定的CdTe量子点与商用的YAG黄光荧光粉混合封装于蓝光LED芯片上,获得RYB三光色复合白光LED,有效地提高了光谱中红光的成分,改善了YAG的显色性,显色指数从原来的62.6提高到了75。其次,将红光发射的Cd(1-x)MnxTe量子点作为荧光粉封装于近紫外发光的LED芯片上,获得发光性能较好的红光量子点LED,说明Cd(1-x)MnxTe量子点可用于LED的封装。并且考察了将少量的Cd(1-x)MnxTe量子点加入到商业YAG黄色荧光粉中,弥补商业YAG荧光粉的缺陷,提高商业用白光LED的发光性能,将显色指数从原来的62.6提高到了78,这比单核CdTe量子点的效果更佳。最后,将ZnCdTe/CdSe核／壳型量子点作为荧光粉封装在蓝光LED芯片上,获得20mA工作电流下显色指数为51.1的白光LED；由于ZnCdTe/CdSe量子点白光LED缺乏绿光的成分导致显色指数低,为了提高其显色指数,将绿光发射的Ca8Mg(SiO4)4Cl2:Eu2+荧光粉与ZnCdTe/CdSe量子点按照合适的比例混合均匀封装在蓝光LED芯片上,获得显示指数较高的白光LED。当Ca8Mg(SiO4)4Cl2:Eu2+荧光粉与ZnCdTe/CdSe量子点的质量比为1：1.5时,获得20mA工作电流下显色指数为88.2的优质白光LED。
(6)通过离子交换法,用Y型分子筛作为主体材料,成功的合成了CdTe/Y纳米复合材料,并讨论了实验条件对合成CdTe/Y纳米复合材料的影响及其合成样品的光催化性能。结果表明,CdTe纳米粒子的负载并没有改变主体分子筛材料的骨架结构,并且所合成的CdTe/Y催化剂具有较好的光催化性能,在紫外光照30分钟时,对甲基蓝的最高降解率达到了87.7%。
White light-emitting diodes (LEDs) is considered as a new generation solid lighting source because of their advantages, such as long service life, high efficiency and environmental protection. At present, the mostly method to realize white LED is the phosphor-converted-LED (pc-LED), which coats the yellow light-emitting phosphor, Y3Al5O12:Ce3+(YAG:Ce) on a blue LED chip. Although this type of white LED has been commercialized, it exhibits low luminous efficiency and low color rendering index (CRI) because of its red spectral deficiency. Therefore, to find a fluorescent material with high luminous efficiency and good stability will become a research hotspot in the white light LED. Quantum Dots (QDs) is a new-style nanometer materials exhibiting distinctive photoluminescence (PL) properties due to the quantum confinement effect. Having many advantages over organic dyes, such as broad excitation, color-tunable, resistance to photobleaching and so on. At present, the excellent properties show great promise for use in the fields of biomedicine, light-emitting diodes (LEDs), solar cells, catalysis and other prospects. Most commercial quantum dots are synthesized by the traditional organic metal method, but the synthesis process with large toxicity. In this study, according to the requirements of applications, our research was mainly focused on the greener synthesis route of quantum dots for light-emitting diodes in an aqueous system. The crystalline structure, component, morphology and size, and optical properties of as-prepared QDs were characterized via X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM), Energy dispersive spectrometer (EDS), photoluminescence spectrum (PL), and UV-Vis absorption spectrum (UV-Vis), respectively. A part of as-prepared quantum dots were used as phosphor for white LED, and the performance of the fabricated W-LED was evaluated. In addition, CdTe/Y nanocomposites were synthesised in an ion exchange method using zeolites Y as hosts. The photocatalytic activities of the CdTe/Y nanocomposites were also investigated systematically. The main contributions were as follows:
(1) Cysteamine (CA)-CdTe QDs were successfully synthesized using a one-step aqueous method. XRD and TEM results show that CdTe QDs with CA modification exhibit a zinc-blended crystal structure in a sphere-like shape. The maximum emission wavelength of CdTe quantum dots could be changed by controlling the reaction time, and the results show that the maximum emission peak exhibited an evident red shift with increasing reflux time due to the quantum size effect. The influences of the reflux temperature, the precursor Cd/Te molar ratios and the pH of the original solution on the luminescence property of the obtained CdTe QDs were investigated systematically. An optimization program of synthesis CdTe QDs was obtained:the precursor Cd/Te molar ratio is1:0.05, the pH of the original solution is5.85, and the reflux temperature is100℃, with a maximum photoluminescence QY of10.73%.
(2) A series of Mn-doped CdTe nanocrystals (NCs) with different concentration of Mn ion were synthesised through a one-step approach in an aqueous medium using thioglycollic acid (TGA) as stabilizer. The obtained Mn-doped CdTe nanocrystals were consistent with the zinc-blended CdTe crystal structure, with approximately spherical aspect of about3.0nm. A red-shift in the emission peak wavelength was observed by doping Mn2+ions into the CdTe QDs to substitute some Cd2+ions. Therefor, the red emission QDs will be more likely obtained by doping Mn2+ions into the CdTe QDs, and red emission QDs is a promising candidate that can be applied in WLEDs.
(3) The obtained CdTe QDs using Na2TeO3as Te source, and three different sulfhydryl compound as ligands, namely tiopronin (TP), L-cysteine (Cys) and mercaptosuccinic acid (MSA). The as-synthesis CdTe with different ligands were zinc-blended structure and approximately spherical. In an aqueous medium, the size-distribution and growth rate of CdTe quantum dots (QDs) are shown to depend on the type of ligands. The growth rate of MSA coated QDs are faster than Cys-and TP-coated QDs. The maximum emission wavelength of MSA-CdTe QDs up to650nm, while the TP-CdTe QDs was586nm at the refluxing time was7h. So larger-size QDs can be synthesized more easily when MSA is chosen as ligand.
(4) A one-step of blue light emission cysteine-capped ZnxCd(1-x)Te alloy QDs has been accomplished by reacting a mixture of ZnCl2and CdCl2with TeO2and using cysteine as surface-stabilizing agent. Without changing the particle size, the fluorescence emissions of QDs can be determined by controlling the Zn2+/Cd2+molar ratio. An evident blue shift was exhibited on the maximum emission peak with increasing the Zn molar ration in the mixture. The ZnxCd(1-X)Te alloy QDs had a blue emission when the Zn/Cd molar ratio was fixed at70:2. The ZnxCd(1-x)Te alloy QDs surface were modified by growth a thin CdSe semiconductor shell on the outer surface of the ZnCdTe NCs. The yellow emission ZnCdTe/CdSe core-shell nanocrystals were prepared to use for white LED.
(5) The RYB "three-band" white LED was fabricated by combining a blue InGaN chip with YAG:Ce and MPA-CdTe QDs used as hybrid phosphors. The WLED showed improved color rendering of light in red with color rendering index (CRI) was increased from62.2to75under20mA forward bias current. A red-light QDs-LED was obtained by encapsulating the red-emiting Cd(1-x)MnxTe onto a blue LED chip, which proved the Cd(1-x)MnxTe QDs available for LED application. Then the white LED was fabricated by combining a blue InGaN chip with YAG:Ce and Cd(1-x)MnxTe QDs used as hybrid phosphors. Because the enhancement of the red spectrum from Cd(1-x)MnxTe QDs can broaden the white emission band, the resultant CRI increased to78at20mA, which is better than single core CdTe QDs. The other white LED consisted of ZnCdTe/CdSe QDs as the phosphor with a blue InGaN chip as the excitation source and showed a low color rendering index (CRI) of51.1caused by the lack of green emissions under a working current of20mA. White LED with a high CRI was obtained with the addition of Ca8Mg(SiO4)4Cl2:Eu2+phosphor, and the CRI of the hybridphosphor white LED was improved to88.2when the mass ratio of Ca8Mg(SiO4)4Cl2:Eu2+phosphor and ZnCdTe/CdSe QDs was1:1.5.
(6) The CdTe/Y nanocomposites were successful synthesized through the ion exchange method, using zeolite Y as host material. The influences of the experimental conditions on photocatalytic activity of the CdTe/Y were investigated systematically. The results showed that the framework structure of zeolite Y was not destroyed and that CdTe QDs were successfully introduced into zeolite Y. Approximately87.7%degradation rate was achieved within30min of irradiation of20mg·L-1methyl blue solution in the presence of CdTe/Y under UV light.
(1)在水相体系中,通过一步水相法成功地合成了巯基乙胺(CA)稳定的CdTe量子点。CA-CdTe量子点为近球形的闪锌矿结构；通过控制体系的反应时间来调节CdTe量子点的发射波长,结果表明,随着回流时间的延长,其最大荧光发射波长发生明显的红移现象,表现出明显的量子尺寸效应。通过对反应温度、前驱体溶液的pH值、Cd与Te的物质的量比等条件的优化,得到了一个巯基乙胺稳定CdTe量子点水相合成的最优合成方案：n(Cd):n (Te2-):n(CA)=1:0.05:2,pH为5.85,温度为100℃,并且最大荧光量子产率可以达到10.73%。
(2)用巯基乙酸作为稳定剂,通过一锅水相法成功地合成了一系列不同Mn离子量掺杂的CdTe纳米粒子。XRD和HRTEM结果表明,样品具有闪锌矿结构CdTe量子点的特征峰,说明Mn离子的加入并没有改变CdTe量子点的晶体结构；并且样品为近球型形状,直径约为3nm。Mn离子的加入使得CdTe量子点的荧光发射光谱发生明显的红移现象,使得更加容易得到红光发射的量子点,可将其应用于商业白光LED以弥补商业荧光粉的缺陷。
(3)以Na2TeO3为碲源,分别以硫普罗宁(TP)、L-半胱氨酸(Cys)和巯基丁二酸(MSA)作为稳定剂,在水相体系中合成水溶性的CdTe量子点。XRD和HRTEM结果表明三种不同稳定剂稳定的CdTe量子点都呈球状的闪锌矿结构,且分散均匀。实验结果表明,分别用三种稳定剂稳定的CdTe量子点均在碱性条件下合成,并且稳定剂的种类对量子点在水相介质中的尺寸分布和生长率有很大的影响。从它们的荧光发射峰可以看出,MSA稳定的CdTe量子点的生长速度最快,当回流到7h时其最大荧光发射达到了650nm的红光发射。TP稳定的CdTe量子点的生长速度最慢,当回流7h时的最强发射波长只有586nm。
(4)分别以ZnCl2、CdCl2、TeO2为Zn源,Cd源和Te源,采用一锅水相法合成水溶性蓝光发射的ZnxCd(1-x)Te量子点。实验结果表明,通过改变Zn2+/Cd2+摩尔比可以调节合金化合物的发光颜色。随着Zn2+/Cd2+摩尔比的增加,ZnxCd(1-x)Te合金型量子点的发射波长发生明显的蓝移现象,当Zn2+/Cd2+摩尔比为70：2时,ZnxCd(1-x)Te合金型量子点发出460nm左右的蓝光。通过对实验合成的ZnCdTe量子点的表面进行修饰,在ZnCdTe量子点的外表面再生长一层CdSe量子点壳,生成黄光发射的ZnCdTe/CdSe核／壳型纳米晶体,可作为白光LED用黄色荧光粉。
(5)采用荧光转换法,用单核的巯基丙酸(MPA)稳定的CdTe量子点与商用的YAG黄光荧光粉混合封装于蓝光LED芯片上,获得RYB三光色复合白光LED,有效地提高了光谱中红光的成分,改善了YAG的显色性,显色指数从原来的62.6提高到了75。其次,将红光发射的Cd(1-x)MnxTe量子点作为荧光粉封装于近紫外发光的LED芯片上,获得发光性能较好的红光量子点LED,说明Cd(1-x)MnxTe量子点可用于LED的封装。并且考察了将少量的Cd(1-x)MnxTe量子点加入到商业YAG黄色荧光粉中,弥补商业YAG荧光粉的缺陷,提高商业用白光LED的发光性能,将显色指数从原来的62.6提高到了78,这比单核CdTe量子点的效果更佳。最后,将ZnCdTe/CdSe核／壳型量子点作为荧光粉封装在蓝光LED芯片上,获得20mA工作电流下显色指数为51.1的白光LED；由于ZnCdTe/CdSe量子点白光LED缺乏绿光的成分导致显色指数低,为了提高其显色指数,将绿光发射的Ca8Mg(SiO4)4Cl2:Eu2+荧光粉与ZnCdTe/CdSe量子点按照合适的比例混合均匀封装在蓝光LED芯片上,获得显示指数较高的白光LED。当Ca8Mg(SiO4)4Cl2:Eu2+荧光粉与ZnCdTe/CdSe量子点的质量比为1：1.5时,获得20mA工作电流下显色指数为88.2的优质白光LED。
(6)通过离子交换法,用Y型分子筛作为主体材料,成功的合成了CdTe/Y纳米复合材料,并讨论了实验条件对合成CdTe/Y纳米复合材料的影响及其合成样品的光催化性能。结果表明,CdTe纳米粒子的负载并没有改变主体分子筛材料的骨架结构,并且所合成的CdTe/Y催化剂具有较好的光催化性能,在紫外光照30分钟时,对甲基蓝的最高降解率达到了87.7%。
White light-emitting diodes (LEDs) is considered as a new generation solid lighting source because of their advantages, such as long service life, high efficiency and environmental protection. At present, the mostly method to realize white LED is the phosphor-converted-LED (pc-LED), which coats the yellow light-emitting phosphor, Y3Al5O12:Ce3+(YAG:Ce) on a blue LED chip. Although this type of white LED has been commercialized, it exhibits low luminous efficiency and low color rendering index (CRI) because of its red spectral deficiency. Therefore, to find a fluorescent material with high luminous efficiency and good stability will become a research hotspot in the white light LED. Quantum Dots (QDs) is a new-style nanometer materials exhibiting distinctive photoluminescence (PL) properties due to the quantum confinement effect. Having many advantages over organic dyes, such as broad excitation, color-tunable, resistance to photobleaching and so on. At present, the excellent properties show great promise for use in the fields of biomedicine, light-emitting diodes (LEDs), solar cells, catalysis and other prospects. Most commercial quantum dots are synthesized by the traditional organic metal method, but the synthesis process with large toxicity. In this study, according to the requirements of applications, our research was mainly focused on the greener synthesis route of quantum dots for light-emitting diodes in an aqueous system. The crystalline structure, component, morphology and size, and optical properties of as-prepared QDs were characterized via X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high resolution transmission electron microscopy (HRTEM), Energy dispersive spectrometer (EDS), photoluminescence spectrum (PL), and UV-Vis absorption spectrum (UV-Vis), respectively. A part of as-prepared quantum dots were used as phosphor for white LED, and the performance of the fabricated W-LED was evaluated. In addition, CdTe/Y nanocomposites were synthesised in an ion exchange method using zeolites Y as hosts. The photocatalytic activities of the CdTe/Y nanocomposites were also investigated systematically. The main contributions were as follows:
(1) Cysteamine (CA)-CdTe QDs were successfully synthesized using a one-step aqueous method. XRD and TEM results show that CdTe QDs with CA modification exhibit a zinc-blended crystal structure in a sphere-like shape. The maximum emission wavelength of CdTe quantum dots could be changed by controlling the reaction time, and the results show that the maximum emission peak exhibited an evident red shift with increasing reflux time due to the quantum size effect. The influences of the reflux temperature, the precursor Cd/Te molar ratios and the pH of the original solution on the luminescence property of the obtained CdTe QDs were investigated systematically. An optimization program of synthesis CdTe QDs was obtained:the precursor Cd/Te molar ratio is1:0.05, the pH of the original solution is5.85, and the reflux temperature is100℃, with a maximum photoluminescence QY of10.73%.
(2) A series of Mn-doped CdTe nanocrystals (NCs) with different concentration of Mn ion were synthesised through a one-step approach in an aqueous medium using thioglycollic acid (TGA) as stabilizer. The obtained Mn-doped CdTe nanocrystals were consistent with the zinc-blended CdTe crystal structure, with approximately spherical aspect of about3.0nm. A red-shift in the emission peak wavelength was observed by doping Mn2+ions into the CdTe QDs to substitute some Cd2+ions. Therefor, the red emission QDs will be more likely obtained by doping Mn2+ions into the CdTe QDs, and red emission QDs is a promising candidate that can be applied in WLEDs.
(3) The obtained CdTe QDs using Na2TeO3as Te source, and three different sulfhydryl compound as ligands, namely tiopronin (TP), L-cysteine (Cys) and mercaptosuccinic acid (MSA). The as-synthesis CdTe with different ligands were zinc-blended structure and approximately spherical. In an aqueous medium, the size-distribution and growth rate of CdTe quantum dots (QDs) are shown to depend on the type of ligands. The growth rate of MSA coated QDs are faster than Cys-and TP-coated QDs. The maximum emission wavelength of MSA-CdTe QDs up to650nm, while the TP-CdTe QDs was586nm at the refluxing time was7h. So larger-size QDs can be synthesized more easily when MSA is chosen as ligand.
(4) A one-step of blue light emission cysteine-capped ZnxCd(1-x)Te alloy QDs has been accomplished by reacting a mixture of ZnCl2and CdCl2with TeO2and using cysteine as surface-stabilizing agent. Without changing the particle size, the fluorescence emissions of QDs can be determined by controlling the Zn2+/Cd2+molar ratio. An evident blue shift was exhibited on the maximum emission peak with increasing the Zn molar ration in the mixture. The ZnxCd(1-X)Te alloy QDs had a blue emission when the Zn/Cd molar ratio was fixed at70:2. The ZnxCd(1-x)Te alloy QDs surface were modified by growth a thin CdSe semiconductor shell on the outer surface of the ZnCdTe NCs. The yellow emission ZnCdTe/CdSe core-shell nanocrystals were prepared to use for white LED.
(5) The RYB "three-band" white LED was fabricated by combining a blue InGaN chip with YAG:Ce and MPA-CdTe QDs used as hybrid phosphors. The WLED showed improved color rendering of light in red with color rendering index (CRI) was increased from62.2to75under20mA forward bias current. A red-light QDs-LED was obtained by encapsulating the red-emiting Cd(1-x)MnxTe onto a blue LED chip, which proved the Cd(1-x)MnxTe QDs available for LED application. Then the white LED was fabricated by combining a blue InGaN chip with YAG:Ce and Cd(1-x)MnxTe QDs used as hybrid phosphors. Because the enhancement of the red spectrum from Cd(1-x)MnxTe QDs can broaden the white emission band, the resultant CRI increased to78at20mA, which is better than single core CdTe QDs. The other white LED consisted of ZnCdTe/CdSe QDs as the phosphor with a blue InGaN chip as the excitation source and showed a low color rendering index (CRI) of51.1caused by the lack of green emissions under a working current of20mA. White LED with a high CRI was obtained with the addition of Ca8Mg(SiO4)4Cl2:Eu2+phosphor, and the CRI of the hybridphosphor white LED was improved to88.2when the mass ratio of Ca8Mg(SiO4)4Cl2:Eu2+phosphor and ZnCdTe/CdSe QDs was1:1.5.
(6) The CdTe/Y nanocomposites were successful synthesized through the ion exchange method, using zeolite Y as host material. The influences of the experimental conditions on photocatalytic activity of the CdTe/Y were investigated systematically. The results showed that the framework structure of zeolite Y was not destroyed and that CdTe QDs were successfully introduced into zeolite Y. Approximately87.7%degradation rate was achieved within30min of irradiation of20mg·L-1methyl blue solution in the presence of CdTe/Y under UV light.
引文
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