微反应器法制备高性能稀土掺杂纳米发光颗粒及其成核生长过程控制
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摘要
无机纳米发光颗粒在免疫生物学和临床检验学等研究领域中体现了极大的潜在应用价值。这类标记物主要包括半导体荧光量子点(Quantum Dots,QDs)及稀土掺杂纳米发光颗粒。目前研究较多的QDs如CdS,CdSe,CdTe等多为有机合成,制备条件苛刻,且本身存在光闪烁、重金属毒性等缺点,限制了其在生物标记上的应用。稀土掺杂纳米发光颗粒具有毒性低、Stokes位移宽,且对光漂白、闪烁以及光化学降解有较强的抵抗性等优势,因而在生物荧光标记上有着巨大的应用潜能。但目前传统方法制备的稀土掺杂纳米发光颗粒存在粒径分布宽、尺寸大、分散性差、发光效率不高等缺陷,难以达到生物荧光标记应用的可再分散、水溶性和发光性能良好等的要求。
本文利用微流体反应器水相合成了LaF_3/LaPO_4:Ln~(3+)(Ln~(3+)=Ce~(3+),Tb~(3+),Eu~(3+)、)纳米发光颗粒,结合微流体力学控制了纳米颗粒在微空间中的成核生长过程;通过优化工艺提高了纳米颗粒的可再分散性、水溶性及荧光性能,并通过微波辐射加热提高了微反应器合成纳米颗粒的产率。全文主要研究工作如下:
(1)利用内径为300μm的聚四氟乙烯微细管作微流体反应器,以醇类试剂(乙二醇(EG)和一缩二乙二醇(DEG)等)为溶剂,在较低反应温度(80～140℃),较短反应时间(5～60 s)内合成稀土掺杂纳米发光颗粒。通过X射线衍射(XRD),透射电子显微镜(TEM),傅立叶变换红外光谱(FTIR Spectrum),紫外可见吸收光谱(UV-Vis Absorption)和荧光光谱(PL Spectrum)等手段对所制备的纳米发光颗粒的结构和性能进行了表征,结果证明用微流体反应器所合成的纳米发光颗粒在结构和性能上都比传统制备方法有了显著提高。
(2)基于高温快速成核和低温较慢生长的结晶理论,设计了两步法微流体反应器,并合成了稀土掺杂纳米发光颗粒。通过表征表明:两步法合成的LaF_3:Ce,Tb纳米发光颗粒具有较窄的粒径分布,粒径在4～5 nm,且表现出优异的水溶性和可再分散性;荧光性能得到了明显提高,尤其是荧光量子产率相对于传统制备方法获得样品有了显著提高,达到了49%。
(3)采用微波辐射对微流体反应段加热,控制成核与生长过程,一步获得稀土掺杂纳米发光颗粒。经表征发现,微波辐射加热微反应器所合成的纳米颗粒在结晶性、分散性以及形貌控制上得到了显著的改进:获得LaF_3:Ce,Tb单分散纳米颗粒的平均粒径为4.5 nm,LaPO_4:Ce,Tb纳米棒的平均长度为65 nm,平均直径为12 nm;两个体系都表现出优异的可再分散性和水溶性;尤其是荧光性能和量子产率,都比油浴恒温加热获得的样品有明显提高。另外,利用微波辐射技术,解决了微流体反应器制备纳米颗粒产率低的问题:获得的Ce~(3+),Tb~(3+)共掺杂LaF_3纳米颗粒和LaPO_4纳米颗粒的产率分别达到了72.3%和91.2%。在微波辅助合成的LaPO_4:Eu纳米颗粒中,发现了由几个纳米单晶组成的25～30 nm大小的纳米颗粒粒组,并呈单分散状,在组内产生显著取向的现象;说明微波辐射对微流体反应器内的结晶过程具有特殊的作用。
(4)为解决提高Eu~(3+)离子掺杂LaF_3纳米颗粒荧光性能的难点,设计了微流体反应器并连续合成了LaF_3:Eu@LaF_3(Core@Shell)核壳结构纳米颗粒。结果表明,在平均粒径为4.5 nm的LaF_3:Eu核粒子表面包覆了一层1.5 nm左右厚的LaF_3基质材料,形成了粒径为6nm核壳结构的纳米颗粒,并使颗粒的结晶性、水溶性及荧光性能得到了显著提高。
Inorganic fluorescent nanocrystals(NCs) show great potential in applications at research fields of immunobiology and clinical examination.Quantum dots(QDs) and lanthanide-doped fluorescent NCs are the two main kinds in these NCs.The QDs, such as CdS,CdSe,CdTe,are mostly prepared in organic phase with harsh conditions. What's more,they could hardly be used in bio-labeling because of the emissiontwinkling and heavy metal toxicity.The lanthanide-doped fluorescent NCs exhibit huge potential applications in bio-labeling because of the low-toxicity,wide Stokes-shift,high resistance to the photobleaching,emission-twinkling and photodegradation.However,the lanthanide-doped NCs produced by the conventional methods usually have wide size distribution,large diameter,poor dispersibility and low emission yield.They could hardly meet the requirements of bio-labeling,which need excellent redispersibility,well water-solubility,and strong emission intensity.
In this paper,LaF_3/LaPO_4:Ln~(3+)(Ln~(3+)=Ce~(3+),Tb~(3+),Eu~(3+)) fluorescent NCs were prepared by microfluidic reactor in aqueous phase.The nucleation and growth processes were controlled in the microspace by microfluidic reactor combined with microfluid dynamics.The redispersibility,water-solubility and the fluorescent intensity were enhanced by optimizing the process in microreactor.The yields of NCs synthesized by microfluidic reactor were improved obviously by microwave irradiation.The studies finished are as follows:
(1) The lanthanide-doped fluorescent NCs were synthesized by a microfluidic reactor made by a Teflon microcapillary with an inside diameter of 300μm.The ethylene glycol(EG) and the diethylene glycol(DEG) were used as the solvents,the reaction temperature is from 80℃to 140℃and the residence time in microcapillary is from 5 s to 60 s.X-Ray Diffraction(XRD),Transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR), UV-vis absorption spectroscopy and Photo-luminescence(PL) spectra were used to characterize the NCs.The results confirmed that the crystalinity and the performances were improved by microfluidic reactor.
(2) Based on the classic crystallization theory,including the momentary nucleation at a high temperature and the slower growth at a lower temperature,the microfluidic reactor was designed as a two-steps path for preparing the lanthanide-doped fluorescent NCs.The results displayed the LaF_3:Ce,Tb NCs prepared by two-step microreactor had a narrow size distribution,about 4～5 nm,excellent redispersibility and water-solubility.The emission intensity was improved obviously.Another attractive improvement was that the quantum yield of the NCs has been improved to 49%,much higher than that by conventional methods.
(3) The microwave(MW) irradiation was used to heat the microfluidic reacting section to control the nucleation and growth processes.The lanthanide-doped fluorescent NCs were obtained by one-step synthesis in microfluidic reactor.The obtained NCs revealed great improvements in crystallinity,dispersibility and shape control by microfluidic reactor under MW irradiation.The monodispersed LaF_3:Ce,Tb nanoparticles had a mean diameter of 4.5 nm,and the LaPO_4:Ce,Tb nanorods had a mean length of 65 nm and diameter of 12 nm.The two systems showed great redispersibility and water-solubility,with obvious improved fluorescent intensity and quantum yields compared to those by oilbath(OB) heating.What's more,the difficulty of how to improve the low yield in microreactor was handled by MW irradiation,LaF_3:Ce,Tb NCs showed a yield of 72.3%and the LaPO_4:Ce,Tb NCs 91.2%.For LaPO_4:Eu NCs,MW irradiation had special effects during the crystallization process.The monodispersed NCs-clusters in which 7～8 little NCs linked together as one had the same tropism.The size was from 25 nm to 30 nm.
(4) LaF_3:Eu@LaF_3 core@ shell NCs were synthesized in a continual microfluidic reactor targeted at the difficulty of how to improve the fluorescent intensity of Eu~(3+) doped LaF_3 NCs.As a result,about a 1.5 nm LaF_3 host material was coated around a LaF_3:Eu core particle with a mean diameter of 4.5 nm,to form a core @ shell structure in size of about 6 nm.The crystallinity,water-solubility and the fluorescent intensity were improved obviously.
本文利用微流体反应器水相合成了LaF_3/LaPO_4:Ln~(3+)(Ln~(3+)=Ce~(3+),Tb~(3+),Eu~(3+)、)纳米发光颗粒,结合微流体力学控制了纳米颗粒在微空间中的成核生长过程;通过优化工艺提高了纳米颗粒的可再分散性、水溶性及荧光性能,并通过微波辐射加热提高了微反应器合成纳米颗粒的产率。全文主要研究工作如下:
(1)利用内径为300μm的聚四氟乙烯微细管作微流体反应器,以醇类试剂(乙二醇(EG)和一缩二乙二醇(DEG)等)为溶剂,在较低反应温度(80～140℃),较短反应时间(5～60 s)内合成稀土掺杂纳米发光颗粒。通过X射线衍射(XRD),透射电子显微镜(TEM),傅立叶变换红外光谱(FTIR Spectrum),紫外可见吸收光谱(UV-Vis Absorption)和荧光光谱(PL Spectrum)等手段对所制备的纳米发光颗粒的结构和性能进行了表征,结果证明用微流体反应器所合成的纳米发光颗粒在结构和性能上都比传统制备方法有了显著提高。
(2)基于高温快速成核和低温较慢生长的结晶理论,设计了两步法微流体反应器,并合成了稀土掺杂纳米发光颗粒。通过表征表明:两步法合成的LaF_3:Ce,Tb纳米发光颗粒具有较窄的粒径分布,粒径在4～5 nm,且表现出优异的水溶性和可再分散性;荧光性能得到了明显提高,尤其是荧光量子产率相对于传统制备方法获得样品有了显著提高,达到了49%。
(3)采用微波辐射对微流体反应段加热,控制成核与生长过程,一步获得稀土掺杂纳米发光颗粒。经表征发现,微波辐射加热微反应器所合成的纳米颗粒在结晶性、分散性以及形貌控制上得到了显著的改进:获得LaF_3:Ce,Tb单分散纳米颗粒的平均粒径为4.5 nm,LaPO_4:Ce,Tb纳米棒的平均长度为65 nm,平均直径为12 nm;两个体系都表现出优异的可再分散性和水溶性;尤其是荧光性能和量子产率,都比油浴恒温加热获得的样品有明显提高。另外,利用微波辐射技术,解决了微流体反应器制备纳米颗粒产率低的问题:获得的Ce~(3+),Tb~(3+)共掺杂LaF_3纳米颗粒和LaPO_4纳米颗粒的产率分别达到了72.3%和91.2%。在微波辅助合成的LaPO_4:Eu纳米颗粒中,发现了由几个纳米单晶组成的25～30 nm大小的纳米颗粒粒组,并呈单分散状,在组内产生显著取向的现象;说明微波辐射对微流体反应器内的结晶过程具有特殊的作用。
(4)为解决提高Eu~(3+)离子掺杂LaF_3纳米颗粒荧光性能的难点,设计了微流体反应器并连续合成了LaF_3:Eu@LaF_3(Core@Shell)核壳结构纳米颗粒。结果表明,在平均粒径为4.5 nm的LaF_3:Eu核粒子表面包覆了一层1.5 nm左右厚的LaF_3基质材料,形成了粒径为6nm核壳结构的纳米颗粒,并使颗粒的结晶性、水溶性及荧光性能得到了显著提高。
Inorganic fluorescent nanocrystals(NCs) show great potential in applications at research fields of immunobiology and clinical examination.Quantum dots(QDs) and lanthanide-doped fluorescent NCs are the two main kinds in these NCs.The QDs, such as CdS,CdSe,CdTe,are mostly prepared in organic phase with harsh conditions. What's more,they could hardly be used in bio-labeling because of the emissiontwinkling and heavy metal toxicity.The lanthanide-doped fluorescent NCs exhibit huge potential applications in bio-labeling because of the low-toxicity,wide Stokes-shift,high resistance to the photobleaching,emission-twinkling and photodegradation.However,the lanthanide-doped NCs produced by the conventional methods usually have wide size distribution,large diameter,poor dispersibility and low emission yield.They could hardly meet the requirements of bio-labeling,which need excellent redispersibility,well water-solubility,and strong emission intensity.
In this paper,LaF_3/LaPO_4:Ln~(3+)(Ln~(3+)=Ce~(3+),Tb~(3+),Eu~(3+)) fluorescent NCs were prepared by microfluidic reactor in aqueous phase.The nucleation and growth processes were controlled in the microspace by microfluidic reactor combined with microfluid dynamics.The redispersibility,water-solubility and the fluorescent intensity were enhanced by optimizing the process in microreactor.The yields of NCs synthesized by microfluidic reactor were improved obviously by microwave irradiation.The studies finished are as follows:
(1) The lanthanide-doped fluorescent NCs were synthesized by a microfluidic reactor made by a Teflon microcapillary with an inside diameter of 300μm.The ethylene glycol(EG) and the diethylene glycol(DEG) were used as the solvents,the reaction temperature is from 80℃to 140℃and the residence time in microcapillary is from 5 s to 60 s.X-Ray Diffraction(XRD),Transmission electron microscopy(TEM),Fourier transform infrared spectroscopy(FT-IR), UV-vis absorption spectroscopy and Photo-luminescence(PL) spectra were used to characterize the NCs.The results confirmed that the crystalinity and the performances were improved by microfluidic reactor.
(2) Based on the classic crystallization theory,including the momentary nucleation at a high temperature and the slower growth at a lower temperature,the microfluidic reactor was designed as a two-steps path for preparing the lanthanide-doped fluorescent NCs.The results displayed the LaF_3:Ce,Tb NCs prepared by two-step microreactor had a narrow size distribution,about 4～5 nm,excellent redispersibility and water-solubility.The emission intensity was improved obviously.Another attractive improvement was that the quantum yield of the NCs has been improved to 49%,much higher than that by conventional methods.
(3) The microwave(MW) irradiation was used to heat the microfluidic reacting section to control the nucleation and growth processes.The lanthanide-doped fluorescent NCs were obtained by one-step synthesis in microfluidic reactor.The obtained NCs revealed great improvements in crystallinity,dispersibility and shape control by microfluidic reactor under MW irradiation.The monodispersed LaF_3:Ce,Tb nanoparticles had a mean diameter of 4.5 nm,and the LaPO_4:Ce,Tb nanorods had a mean length of 65 nm and diameter of 12 nm.The two systems showed great redispersibility and water-solubility,with obvious improved fluorescent intensity and quantum yields compared to those by oilbath(OB) heating.What's more,the difficulty of how to improve the low yield in microreactor was handled by MW irradiation,LaF_3:Ce,Tb NCs showed a yield of 72.3%and the LaPO_4:Ce,Tb NCs 91.2%.For LaPO_4:Eu NCs,MW irradiation had special effects during the crystallization process.The monodispersed NCs-clusters in which 7～8 little NCs linked together as one had the same tropism.The size was from 25 nm to 30 nm.
(4) LaF_3:Eu@LaF_3 core@ shell NCs were synthesized in a continual microfluidic reactor targeted at the difficulty of how to improve the fluorescent intensity of Eu~(3+) doped LaF_3 NCs.As a result,about a 1.5 nm LaF_3 host material was coated around a LaF_3:Eu core particle with a mean diameter of 4.5 nm,to form a core @ shell structure in size of about 6 nm.The crystallinity,water-solubility and the fluorescent intensity were improved obviously.
引文
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