磷酸锶、磷酸钙白光LED蓝色荧光粉的合成及发光性能研究
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摘要
白光LED以其独特的特点,如省电、体积小、寿命长、无环境污染、可回收等,受到了广泛的关注。白光LED是继油灯、白炽灯、荧光灯之后的第四代光源,是二十一世纪光源,代表了未来照明产业的发展方向。
随着材料科学技术的发展,一些软化学合成方法,如燃烧法、溶胶-凝胶法、共沉淀法及水热合成法已成功应用在白光LED用荧光粉的合成。燃烧法具有容易、快捷的特点,因而在各种白光LED荧光粉的合成中被广泛应用。而柠檬酸溶胶-凝胶法合成温度低,节约能源,纯度较高,粒度小,可轻松达到纳米级等优点,成为现研究领域中除了传统的高温固相法之外的主流合成方法。
本文采用燃烧法,柠檬酸溶胶-凝胶法合成了磷酸锶、磷酸钙UV-LED及NUV-LED用荧光粉。运用X-射线粉末衍射仪(XRD)、透射电子显微镜(TEM)、荧光/磷光发光分光光度计对荧光粉对晶体结构、形貌、激发和发射光谱进行了分析。主要内容包括:
(1)综述了白光LED的结构和原理,白光LED用荧光粉研究现状,并介绍了影响其发光性能的重要因素。
(2)采用燃烧法制备出了UV-NUVLED用荧光粉α-Sr1.96P2O7:0.04Eu~(2+)。该荧光粉在290nm,330nm和387nm三处被激发,发射光谱为在420 nm的单峰,可作为白光LED蓝光部分。
(3)采用燃烧法合成了NUV-LED用蓝色荧光粉β-Ca1.95P2O7:0.05Eu~(2+)。分别对荧光粉的晶体结构、形貌、激发和发射光谱进行了研究。XRD发现温度到1000℃时,基质晶相发生转变可得到目标产物β-Ca1.95P2O7:0.05Eu~(2+),同时晶体的转变导致了发射峰的红移。TEM结果也证实了这一点。该荧光粉主激发峰为387nm,发射峰单一,在421nm。可在近紫外区得到有效的激发。
(4)采用柠檬酸-溶胶凝胶法制备出了UV-LED用荧光粉Sr_2P_2O_7:Eu~(2+)。研究了燃烧的温度、尿素与硝酸盐的质量比、铕的摩尔分数对荧光粉发光性质的影响,得出了最佳合成条件。结果表明掺Eu~(2+)量为0.05mol,pH=3.0在700℃下煅烧5 h得到的荧光粉发光性能良好,具有较小的尺寸(约20-40 nm)和较好的颗粒形貌。
(5)采用燃烧法合成了UV-NUVLED用蓝粉Ca2(1-y)Sr2yP2O7:Eu~(2+)。利用X射线衍射(XRD)、电子显微镜(TEM)以及荧光/磷光发光分光光度计等手段对Ca2(1-y)Sr2yP2O7:Eu~(2+)荧光粉的物相结构、形貌粒度、发光性质等进行了研究。发现阳离子Sr2+的掺入可显著的提高Ca_2P_2O_7:Eu~(2+)的发射强度。
White light emitting diodes (LEDs) have been paid more and more attention due to their energy conversation, little volume, long service life, pollution-free and high efficiency. White LEDs are believed to be the fourth generation of lamp-house after oil lamp, incandescent lamp and fluorescent light and there are the future of illumination, which have huge market.
With the development of materials science and technology, some soft chemical synthesis methods, such as combustion synthesis methods, sol–gel method, co-precipitation and hydrothermal synthesis methods have been successfully applied to synthesize the white LED phosphors. Combustion synthesis is characterized by more complete reaction, the increased reaction efficiency, fast reaction and convenient. Citrate sol-gel method is one of the most important techniques for the synthesis of various functional materials because citrate sol-gel routes are efcient alternatives as they offer better purity and homogeneity, and can yield stoichiometric powders with smaller grain size particles atrelatively lower processing temperature in comparison with conventional solid-state reaction.
In this paper the combustion method and citrate sol-gel method is applied to synthesized the WLED blue phosphors-Sr_2P_2O_7:Eu~(2+) and Ca_2P_2O_7:Eu~(2+). X-ray diffractometer (XRD), transmission electron microscope (TEM) and luminescence spectrophotometer were used to analyze and measure the crystal structure, morphology, excitation and emission spectra.
The following is included:
(1) The present status and prospect of white LEDs are reviewed firstly. Then it analysises the light emitting principles,the preparation methods, influence factors of white LED phosphores were introduced.
(2) The blue-emitting phosphorα-Sr1.96P2O7:0.04Eu~(2+) was prepared by combustion method as the fluorescent material for white light emitting diodes (WLEDs). The emission spectrum shows a single intense band centered at 417 nm, the excitation spectrum is a broad band with three bands centered at 290 nm, 328 nm and 387 nm, which matches the emission of ultraviolet light emitting diodes (UV-LEDs).
(3) The blue light emitting phosphor,β-Ca1.95P2O7:0.05Eu~(2+), was prepared by combustion method. From the results of XRD, it is found that the matrix underwent phase transformation at 1000℃. Phase transition result the red shift of the emission peak of about 9 nm. This phenomenon has been confirmed in the TEM results. The emission spectrum shows a single intense band centered at 421 nm. The excitation spectrum is a broad band extending with two peaks at about 330 and 387 nm. It is shown that theβ-Ca1.95P2O7:0.05Eu~(2+) phosphor can be effectively excitated by near ultraviolet light (370-410nm). The investigated phosphor is suitable for a NUV LED excitation.
(4) The blue emitting phosphor Sr_2P_2O_7:Eu~(2+) has been synthesized by citrate sol-gel method. The sample with pH=3.0 and 0.05mol Eu~(2+) that synthesized at calcining temperature of 700℃for 5h exhibits the excellent luminous properties. The emission spectrum shows a single intense band centered at 417 nm, the excitation spectrum is a broad band extending from 220 nm to 400 nm, the Sr_2P_2O_7:Eu~(2+) is a potential materials for white LEDs.
(5) Blue emitting phosphors Ca2(1-y)Sr2yP2O7:Eu~(2+) have been synthesized by combustion method. X-ray diffractometer, transmission electron microscope and luminescence spectrophotometer were used to analyze and measure the crystal structure, morphology, excitation and emission spectra of the Ca2(1-y)Sr2yP2O7:Eu~(2+) phosphor. It is found that the emisstion intensity of Ca_2P_2O_7:Eu~(2+) enhanced with the doping Sr2+ ions.
随着材料科学技术的发展,一些软化学合成方法,如燃烧法、溶胶-凝胶法、共沉淀法及水热合成法已成功应用在白光LED用荧光粉的合成。燃烧法具有容易、快捷的特点,因而在各种白光LED荧光粉的合成中被广泛应用。而柠檬酸溶胶-凝胶法合成温度低,节约能源,纯度较高,粒度小,可轻松达到纳米级等优点,成为现研究领域中除了传统的高温固相法之外的主流合成方法。
本文采用燃烧法,柠檬酸溶胶-凝胶法合成了磷酸锶、磷酸钙UV-LED及NUV-LED用荧光粉。运用X-射线粉末衍射仪(XRD)、透射电子显微镜(TEM)、荧光/磷光发光分光光度计对荧光粉对晶体结构、形貌、激发和发射光谱进行了分析。主要内容包括:
(1)综述了白光LED的结构和原理,白光LED用荧光粉研究现状,并介绍了影响其发光性能的重要因素。
(2)采用燃烧法制备出了UV-NUVLED用荧光粉α-Sr1.96P2O7:0.04Eu~(2+)。该荧光粉在290nm,330nm和387nm三处被激发,发射光谱为在420 nm的单峰,可作为白光LED蓝光部分。
(3)采用燃烧法合成了NUV-LED用蓝色荧光粉β-Ca1.95P2O7:0.05Eu~(2+)。分别对荧光粉的晶体结构、形貌、激发和发射光谱进行了研究。XRD发现温度到1000℃时,基质晶相发生转变可得到目标产物β-Ca1.95P2O7:0.05Eu~(2+),同时晶体的转变导致了发射峰的红移。TEM结果也证实了这一点。该荧光粉主激发峰为387nm,发射峰单一,在421nm。可在近紫外区得到有效的激发。
(4)采用柠檬酸-溶胶凝胶法制备出了UV-LED用荧光粉Sr_2P_2O_7:Eu~(2+)。研究了燃烧的温度、尿素与硝酸盐的质量比、铕的摩尔分数对荧光粉发光性质的影响,得出了最佳合成条件。结果表明掺Eu~(2+)量为0.05mol,pH=3.0在700℃下煅烧5 h得到的荧光粉发光性能良好,具有较小的尺寸(约20-40 nm)和较好的颗粒形貌。
(5)采用燃烧法合成了UV-NUVLED用蓝粉Ca2(1-y)Sr2yP2O7:Eu~(2+)。利用X射线衍射(XRD)、电子显微镜(TEM)以及荧光/磷光发光分光光度计等手段对Ca2(1-y)Sr2yP2O7:Eu~(2+)荧光粉的物相结构、形貌粒度、发光性质等进行了研究。发现阳离子Sr2+的掺入可显著的提高Ca_2P_2O_7:Eu~(2+)的发射强度。
White light emitting diodes (LEDs) have been paid more and more attention due to their energy conversation, little volume, long service life, pollution-free and high efficiency. White LEDs are believed to be the fourth generation of lamp-house after oil lamp, incandescent lamp and fluorescent light and there are the future of illumination, which have huge market.
With the development of materials science and technology, some soft chemical synthesis methods, such as combustion synthesis methods, sol–gel method, co-precipitation and hydrothermal synthesis methods have been successfully applied to synthesize the white LED phosphors. Combustion synthesis is characterized by more complete reaction, the increased reaction efficiency, fast reaction and convenient. Citrate sol-gel method is one of the most important techniques for the synthesis of various functional materials because citrate sol-gel routes are efcient alternatives as they offer better purity and homogeneity, and can yield stoichiometric powders with smaller grain size particles atrelatively lower processing temperature in comparison with conventional solid-state reaction.
In this paper the combustion method and citrate sol-gel method is applied to synthesized the WLED blue phosphors-Sr_2P_2O_7:Eu~(2+) and Ca_2P_2O_7:Eu~(2+). X-ray diffractometer (XRD), transmission electron microscope (TEM) and luminescence spectrophotometer were used to analyze and measure the crystal structure, morphology, excitation and emission spectra.
The following is included:
(1) The present status and prospect of white LEDs are reviewed firstly. Then it analysises the light emitting principles,the preparation methods, influence factors of white LED phosphores were introduced.
(2) The blue-emitting phosphorα-Sr1.96P2O7:0.04Eu~(2+) was prepared by combustion method as the fluorescent material for white light emitting diodes (WLEDs). The emission spectrum shows a single intense band centered at 417 nm, the excitation spectrum is a broad band with three bands centered at 290 nm, 328 nm and 387 nm, which matches the emission of ultraviolet light emitting diodes (UV-LEDs).
(3) The blue light emitting phosphor,β-Ca1.95P2O7:0.05Eu~(2+), was prepared by combustion method. From the results of XRD, it is found that the matrix underwent phase transformation at 1000℃. Phase transition result the red shift of the emission peak of about 9 nm. This phenomenon has been confirmed in the TEM results. The emission spectrum shows a single intense band centered at 421 nm. The excitation spectrum is a broad band extending with two peaks at about 330 and 387 nm. It is shown that theβ-Ca1.95P2O7:0.05Eu~(2+) phosphor can be effectively excitated by near ultraviolet light (370-410nm). The investigated phosphor is suitable for a NUV LED excitation.
(4) The blue emitting phosphor Sr_2P_2O_7:Eu~(2+) has been synthesized by citrate sol-gel method. The sample with pH=3.0 and 0.05mol Eu~(2+) that synthesized at calcining temperature of 700℃for 5h exhibits the excellent luminous properties. The emission spectrum shows a single intense band centered at 417 nm, the excitation spectrum is a broad band extending from 220 nm to 400 nm, the Sr_2P_2O_7:Eu~(2+) is a potential materials for white LEDs.
(5) Blue emitting phosphors Ca2(1-y)Sr2yP2O7:Eu~(2+) have been synthesized by combustion method. X-ray diffractometer, transmission electron microscope and luminescence spectrophotometer were used to analyze and measure the crystal structure, morphology, excitation and emission spectra of the Ca2(1-y)Sr2yP2O7:Eu~(2+) phosphor. It is found that the emisstion intensity of Ca_2P_2O_7:Eu~(2+) enhanced with the doping Sr2+ ions.
引文
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