PDP用蓝、绿色荧光粉的合成及光谱性质
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摘要
等离子平板显示技术(Plasma flat panel display technology)消除了画面几何变形,具有聚焦清晰、亮度均匀、色彩纯度高、对比度高,画面大、视角宽阔等一系列优点,是高清电视的一个非常重要的发展方向,它已成为最有希望的大屏幕高清晰度的平板显示技术。
荧光粉是决定显示质量的关键因素之一。PDP荧光粉用147nm或172nm的真空紫外线激发,因此,要求其应具备热稳定性好、发光效率高、粉体粒度小、粒径分布范围较窄、色纯度高、余辉时间短等性能。目前,PDP商用荧光粉的性能还存在许多缺陷：(1)红粉：Y2O3:Eu3+发光效率相对比较低,而(Y,Gd)BO3:Eu3+色纯度不高；(2)蓝粉：Eu2+激活的BaMgAl10O17(BAM)荧光粉稳定性差,光色变化大；(3)绿粉：Zn2SiO4:Mn2+余辉时间太长。
基于上述原因,本文利用XRD、SEM、粒度、荧光粉性能分析等手段,对PDP用(La,Ce,Tb)BO3和Ln(BO3,PO4):Ce3+,Tb3+绿色荧光粉的合成与光谱特性、BAM:Eu2+蓝色荧光粉的合成及抗热劣化性能进行了研究；以BAM:Eu2+荧光粉为合成对象,研究了助熔剂对BAM:Eu2+荧光粉合成机理和发光性能的影响；以SrAl2O4:Eu,Dy发光材料为合成对象,对喷雾热解制备稀土发光材料工艺进行了研究,通过实验得出以下结论：
(1)高温固相法合成的(La,Ce,Tb)BO3绿色发光粉的晶体结构和LaBO3相同,Ce3+, Tb3+的掺入没有改变基质晶体结构,发光粉颗粒大小均匀,形貌规则,粒度在5μm左右。随Tb3+含量的增加样品中TbBO3相增加,当Tb含量达15%(mol)及以上时,TbBO3杂相含量增加更为明显。(La,Ce,Tb)BO3的光谱性质表明,在(La,Ce,Tb)BO3的发射和激发光谱中除了有铽的特征发射和激发峰外,还有Ce3+的特征激发峰和发射峰。(La,Tb)BO3的激发光谱和(;La,Ce)BO3发射光谱存在重叠,这为Ce3+→Tb3+的能量传递创造了条件。在(La,Ce,Tb)BO3中存在铈、铽的浓度猝灭效应,固定铈或铽的情况下,增加铽或铈的含量,(La,Ce,Tb)BO3的发射主峰的相对强度均呈先升后降的态势。固定铈铽比时,(La,Ce,Tb)BO3的发射主峰的相对强度随镧的增加先升后降,当镧含量为70%时,发射主峰相对强度最高。镧含量为80%时,在较宽的Ce/Tb范围内,能得到发光性能较好的(La,Ce,Tb)BO3样品。固定镧含量时,当镧含量为80%及以内时,(La,Ce,Tb)BO3的发射主峰的相对强度随Ce/Tb的增大先升后降,当铈铽比为3/1时,(La,Ce,Tb)BO3的发射主峰的相对强度达到最大。对(La,Ce,Tb)BO3的发射谱图与商品粉(La,Ce,Tb)PO4进行了比较,两者的发射主峰都在541nm处,(La,Ce,Tb)BO3在489nm处的发射峰稍有红移,计算表明,(La,Ce,Tb)BO3的发光亮度达到商品粉(La,Ce,Tb)PO4的94.7%,是一很有应用前景的绿色发光粉。
(2)以自制磷酸硼(BP04)及稀土化合物为原料,采用一步烧成法合成了具有良好结晶的Ce3+,Tb3+激活的Ln(BO3,PO4)(Ln=La, Y, Gd)荧光粉,并对其在147nm激发下的光谱性质进行了研究。结果表明：Ln(BO3,PO4):Ce3+,Tb3+(Ln=Y, La, Gd)激发光谱是由来自B033-和P043-的120-175nm基质敏化带和来自Tb3+离子的4f→5d跃迁的175-300nm多宽带组成；改变基质稀土离子,发射光谱中的荧光分支比和色坐标也随之改变,其中以Gd(BO3,PO4):Ce3+,Tb3+荧光粉的荧光分支比为最高；拟合Gd(BO3,PO4):Ce3+,Tb3+荧光粉的衰减曲线后,得出其荧光寿命为2.92ms,10%的余辉为6.7ms,优于Zn2SiO4:Mn2+商品粉,能够满足PDP器件的要求。高温固相一步法是一行之有效的稀土硼酸盐发光材料合成方法,在较低合成温度条件下,便可得到与传统高温固相法晶型结构相同、结晶更完整的样品。高温固相一步法合成的Ln(BO3,PO4):Ce3+,Tb3+荧光粉的发光性能优于传统高温固相法所制备的荧光粉。
(3)采用高温固相法制备了BaMgAl10O17:Eu2+(BAM:Eu2+)蓝色荧光粉。研究表明：合成工艺条件,诸如激活离子浓度、烧结温度和时间、还原温度和时间等,对BAM晶体结晶度、物相纯度、粉体颗粒形貌和发光强度有较大影响；少量Sr取代Ba对基质晶体结构的影响很小,Sr的掺入使BAM蓝粉的相对发光亮度下降,但可以提高其抗热劣化性能。采用实验所获得的较优条件所制备的Ba0.82Sr0.08MgAl10O17:Eu0.1蓝粉粒度为3.24gm,色坐标为x=0.0151、y=0.075(与商品粉的色坐标x=0.0145、y=0.072接近),发光亮度基本相当,相对亮度为商品粉的98.3%,抗热劣化性能优于商品粉,符合PDP用蓝色荧光粉的要求。
采用不同的助熔剂,均能制备出BAM:Eu2+发光材料,且样品的形貌更规整、颗粒大小更趋均一；Eu2+的掺入对基质晶体结构没有明显的影响；随着烧结时间的延长,样品结晶更趋完整、杂相减少,粉体发光强度随之提高；采用不同的助熔剂,合成反应的机理发生变化,所得样品的结晶完整性、杂相组成和含量、发光中心的分布、粉体粒径等性能产生相应变化,最终导致样品的发光性能发生改变,样品的特征发射峰强度随AlF3、H3BO3、 MgF2、Li2CO3、无助熔剂依次降低。
(4)以SrAl2O4:Eu,Dy为合成对象,考察了喷雾热解法合成稀土发光材料的可行性。实验结果表明：只要控制好工艺技术条件,喷雾热解法是一可取的合成稀土发光材料的方法；较之高温固相法,喷雾热解法能在较低的温度下制备具有分散性好、粒度小、粒径分布窄(2μm～5μm)、形貌规则(实心球形)、发光性能优良等优点的发光材料。
喷雾热解两段法制备的SrAl2O4:Eu,Dy发光材料的晶体结构与a-SrAl2O4磷石英晶体结构相同,掺杂Eu、Dy对晶体结构的影响很小。金属离子总浓度、热解温度和还原温度对产物的形貌、粒度分布、发光性能有较大影响。随着还原温度的升高,产物的发射主峰位置发生红移。
添加剂的使用能明显改善和修饰材料的形貌、增强材料的初始亮度、延长材料的余辉时间(柠檬酸的使用会缩短材料的余辉时间)。柠檬酸的加入有助于获得实心球形颗粒,乙醇除了良好的分散性,还能有效的增大颗粒的球形度,但无法获得实心颗粒,PEG能够起到分散剂和稳定剂的作用。当三种添加剂同时使用时可获得初始亮度高、余辉时间长、分散性好、粒度小、粒径分布窄(2μm～5μm)的实心球形颗粒。
Plasma flat panel display technology eliminates the geometric distortion of the picture, and offers brightness uniformity, high color purity, high contrast, and other advantages. Plasma flat panels (PDPs) is the most promising candidate for large size flat-panel information-display devices, is a very important development direction of HDTV. Fluorescent powders are one of the key factors which determine display quality. PDP phosphor is excited by147nm or172nm vuv light, therefore, it should have good thermal stability, high luminous efficiency, small powder particle size, and a narrow range of grain size distribution, high color purity, afterglow time is short and other properties. The performance of present commodities-PDP phosphor has many shortcomings:(l)red phosphor:color purity of (Y,Gd) BO3:Eu3+red phosphor is not high, and light-emitting efficiency of Y2O3:Eu3+is relatively low, and (2)blue phosphor: Eu2+activated BAM phosphor has poor stability, and its peak maximum also shift during various stages of panel fabrication and (3)green powder:the decay time of Zn2SiO4:Mn2+phosphor is somewhat longer for practical application.
Therefore,(La,Ce,Tb) BO3green phosphor, Ln (BO3,PO4):Ce3+,Tb3+green phosphor, BAM:Eu2+blue phosphor for PDP are synthesized by high temperature solid state reaction and modified high temperature solid state reaction. SEM, XRD, TG-DTA, luminescence spectra and other means were used to study the phosphor samples. The effect of flux on high temperature solid state reaction mechanism and the feasibility of the spray pyrolysis synthesis using to synthesize rare earth luminescent materials were studied. The studied conclusions came following:
(1) The phosphors of (La,Ce,Tb)BO3was synthesized by high temperature solid state reaction. X-ray diffractometry (XRD) patterns indicate that the Crystal Structure of (La,Ce,Tb)BO3and LaBO3is the same. The crystal structure has not been changed by Ce3+and Tb3+mixed into. Emission scanning electron microscopy (SEM) images show that the particle size of phosphors is more uniform, morphology is more rules, and granularity is about5μm. The content of TbBO3phase in (La,Ce,Tb)BO3increases with increasing of Tb content in (La,Ce,Tb)BO3. When Tb concentration reaches15%and above, the content of TbBO3phase in (La,Ce,Tb)BO3increases more rapidly. The luminescence properties of (La,Ce,Tb)BO3and the sensitization of Ce3+to Tb3+were studied. There are three peaks at around244,268and330nm in the excitation spectrum of Ce3+, and there are two peaks at365and380nm in the emission spectrum of Ce3+, respectively. All of them have the large overlap. The excitation peaks of Tb3+is230nm and its Maximum emission wavelength is541nm. Both the Tb3+characteristic emission and excitation peaks and the Ce3+characteristic emission and excitation peaks were observed in the emission and excitation spectrum of (La,Ce,Tb)BO3. Comparing the emission spectrum of (La,Tb)BO3with the excitation spectrum of (La,Ce)BO3, and find them having the large overlap, it inferred that there is remarkable energy transfer from Ce3+to Tb3+in it. When the concentration of Ce or Tb in (La,Ce,Tb)BO3is fixed, because of concentration self-quenching effect, the relative intensity of main emission peak (at541nm)increases firstly and then decreases with increasing of the concentration of Tb or Ce. At fixed ratio of Ce concentration to Tb concentration, the relative intensity of the main emission peak of (La,Ce,Tb)BO3is the highest when La concentration in (La,Ce,Tb)BO3reaches70%. The sample with better luminescence properties will be obtained in variety range of Ce concentration to Tb concentration at fixed La concentration of80%. When La concentration is80%and above, the relative intensity of the main emission peak of (La,Ce,Tb)BO3will be highest at Ce concentration to Tb concentration of3/1. Comparing commercial phosphor (La,Ce,Tb)PO4with experimental (La,Ce,Tb)BO3phosphor, experimental (La,Ce,Tb)BO3phosphor has a little red shift at489nm and its relative emission intensity was94.7%of the commercial phosphor (La,Ce,Tb)PO4. Therefore, it is inferred that (La,Ce,Tb)BO3would be a promising PDP green-emitting phosphor.
(2) Cerium-and terbium-doped lanthanum borophosphate [Ln(BO3,PO4):Ce3+, Tb3+] phosphor have been prepared by a single-step calcination using self-made BPO4as borophosphate sourse. Fine crystal structures are observed by XRD patterns. The excitation spectrum of Ln(BO3,PO4):Ce3+,Tb3+(Ln=Y, La, Gd) includes host sensitization band at120-175nm which is relative to the BO33-and PO43-groups, and several bands at175-300nm originated from4f→5d transition of Tb3+. The replacement of the host leads to changes of fluorescence Intensity ratios and CIE coordinate in emission spectrum. Among these phosphors, Gd(BO3,PO4):Ce3+,Tb3+phosphor shows best green fluorescence intensity ratio. The lifetime of the emission transition3D4→7F4of Tb3+is2.92ms, with a10%afterglow of6.7ms, which make it better than Zn2SiO4:Mn2+commercial phosphor for PDP.
(3) BaMgAl10O17:Eu2+phosphors were synthesized by high temperature solid-state reaction method. Using the X-ray powder diffraction, scanning electron microscopy and photoluminescence spectra, the effect of different fluxes, reaction time on such properties as crystals crystallinity, phase purity, particle morphology, luminescence intensity and thermally stability of the blue phosphor were investigated. The mechanism of synthesis of BaMgAl10O17:Eu2+with different fluxes was analyzed. The results show that synthesis conditions such as flux, concentration of doped ions, sintering temperature and time, reduction temperature and time have important influence on crystals crystallinity, phase purity, particle morphology, luminescence intensity and thermally stability of the blue phosphor. Incorporation of Sr has little influence on crystal structure of BAM matrix, it would cause the drop of initial relative brightness of phosphor's, but the thermally stability of BAM luminous phosphor would be improved. When flux is adopted, BaMgAl10O17:Eu2+phosphors with more regular morphology, uniform particle size and crystals crystallinity can be obtained at lower sintering temperature. Incorporation of Eu2+has less influence on crystal structure of BaMgAl10O17matrix. Along with the agglutination time's extension, the sample's crystallization becomes more completely, the content of impurity phase in it reduces and its luminous intensity increase. As different fluxes are used, the mechanism of synthesis of BaMgAl10O17:Eu2+will change. The performances of prepared sample such as crystallization integrity, phase purity, the luminescent center distribution have corresponding change with the change of the synthesis mechanism, thus the luminescent properties of the samples change correspondingly.
Comparing the experimental blue phosphor obtained at optimized conditions (Ba0.82Sr0.08MgAl10O17:Eu0.1) with the commodity powder BAM, relative emission intensity of the experimental blue phosphor is98.3%of the commercial phosphor BAM, its color coordinate is close to the commercial phosphor (experimental blue phosphor's color coordinate is x=0.0145, y=0.072, and the color coordinate of commercial phosphor is x=0.0145, y=0.072). The experimental blue phosphor has better thermally stability than that of the commercial phosphor. The granularity of it was3.24μm Therefore, it is expected that the experimental blue phosphor would be used for PDP blue phosphor.
(4) Through the synthesis of SrAl2O4:Eu,Dy, the feasibility of the spray pyrolysis synthesis using to synthesize rare earth luminescent materials was studied. Experimental results show that spray pyrolysis method is a desirable method of synthesis of rare earth luminescence materials as long as the technology conditions are optimized. Compared with the SrAl2O4:Eu,Dy prepared by solid state method, the SrAl2O4:Eu,Dy prepared by spray pyrolysis has more regular morphology (compact solid spherical particles), smaller particle size, narrower particle size distribution and more excellent luminescent properties, and the synthesis temperature can be significantly reduced.
The SrAl2O4:Eu,Dy prepared by spray pyrolysis belongs to the α-SrAl2O4phosphor crystal structure and small amount of Eu, Dy doped into the matrix has little effect on the crystal structure of SrAl2O4. The morphology, size distribution and luminous performances of the phosphors could be affected with synthesizing conditions, such as precursor concentration, sintering temperature, reduction temperature etc. As the reduction temperature rised, red shift of the main peak position in the emission spectrum occurs (move to longer wavelengths).
Additives caould obviously improve the morphology, reinforce the initial brightness, and enlarge the afterlow time (citric acid would shorten the afterlow time). Citric acid could help to obtain solid spherical particle. Ethanol was not only a good dispersant but also improved the sphericity of particle. Howerve, solid spherical particles couldn't be gotten in this condition. PEG played the role of dispersant and stabilizer. The solid spherical SrAl2O4:Eu,Dy particles with high initial brightness, long twilight time, good dispersion, small particle size and narrow particle size distribution (2μm～5μm) when these additives was used at the same time.
荧光粉是决定显示质量的关键因素之一。PDP荧光粉用147nm或172nm的真空紫外线激发,因此,要求其应具备热稳定性好、发光效率高、粉体粒度小、粒径分布范围较窄、色纯度高、余辉时间短等性能。目前,PDP商用荧光粉的性能还存在许多缺陷：(1)红粉：Y2O3:Eu3+发光效率相对比较低,而(Y,Gd)BO3:Eu3+色纯度不高；(2)蓝粉：Eu2+激活的BaMgAl10O17(BAM)荧光粉稳定性差,光色变化大；(3)绿粉：Zn2SiO4:Mn2+余辉时间太长。
基于上述原因,本文利用XRD、SEM、粒度、荧光粉性能分析等手段,对PDP用(La,Ce,Tb)BO3和Ln(BO3,PO4):Ce3+,Tb3+绿色荧光粉的合成与光谱特性、BAM:Eu2+蓝色荧光粉的合成及抗热劣化性能进行了研究；以BAM:Eu2+荧光粉为合成对象,研究了助熔剂对BAM:Eu2+荧光粉合成机理和发光性能的影响；以SrAl2O4:Eu,Dy发光材料为合成对象,对喷雾热解制备稀土发光材料工艺进行了研究,通过实验得出以下结论：
(1)高温固相法合成的(La,Ce,Tb)BO3绿色发光粉的晶体结构和LaBO3相同,Ce3+, Tb3+的掺入没有改变基质晶体结构,发光粉颗粒大小均匀,形貌规则,粒度在5μm左右。随Tb3+含量的增加样品中TbBO3相增加,当Tb含量达15%(mol)及以上时,TbBO3杂相含量增加更为明显。(La,Ce,Tb)BO3的光谱性质表明,在(La,Ce,Tb)BO3的发射和激发光谱中除了有铽的特征发射和激发峰外,还有Ce3+的特征激发峰和发射峰。(La,Tb)BO3的激发光谱和(;La,Ce)BO3发射光谱存在重叠,这为Ce3+→Tb3+的能量传递创造了条件。在(La,Ce,Tb)BO3中存在铈、铽的浓度猝灭效应,固定铈或铽的情况下,增加铽或铈的含量,(La,Ce,Tb)BO3的发射主峰的相对强度均呈先升后降的态势。固定铈铽比时,(La,Ce,Tb)BO3的发射主峰的相对强度随镧的增加先升后降,当镧含量为70%时,发射主峰相对强度最高。镧含量为80%时,在较宽的Ce/Tb范围内,能得到发光性能较好的(La,Ce,Tb)BO3样品。固定镧含量时,当镧含量为80%及以内时,(La,Ce,Tb)BO3的发射主峰的相对强度随Ce/Tb的增大先升后降,当铈铽比为3/1时,(La,Ce,Tb)BO3的发射主峰的相对强度达到最大。对(La,Ce,Tb)BO3的发射谱图与商品粉(La,Ce,Tb)PO4进行了比较,两者的发射主峰都在541nm处,(La,Ce,Tb)BO3在489nm处的发射峰稍有红移,计算表明,(La,Ce,Tb)BO3的发光亮度达到商品粉(La,Ce,Tb)PO4的94.7%,是一很有应用前景的绿色发光粉。
(2)以自制磷酸硼(BP04)及稀土化合物为原料,采用一步烧成法合成了具有良好结晶的Ce3+,Tb3+激活的Ln(BO3,PO4)(Ln=La, Y, Gd)荧光粉,并对其在147nm激发下的光谱性质进行了研究。结果表明：Ln(BO3,PO4):Ce3+,Tb3+(Ln=Y, La, Gd)激发光谱是由来自B033-和P043-的120-175nm基质敏化带和来自Tb3+离子的4f→5d跃迁的175-300nm多宽带组成；改变基质稀土离子,发射光谱中的荧光分支比和色坐标也随之改变,其中以Gd(BO3,PO4):Ce3+,Tb3+荧光粉的荧光分支比为最高；拟合Gd(BO3,PO4):Ce3+,Tb3+荧光粉的衰减曲线后,得出其荧光寿命为2.92ms,10%的余辉为6.7ms,优于Zn2SiO4:Mn2+商品粉,能够满足PDP器件的要求。高温固相一步法是一行之有效的稀土硼酸盐发光材料合成方法,在较低合成温度条件下,便可得到与传统高温固相法晶型结构相同、结晶更完整的样品。高温固相一步法合成的Ln(BO3,PO4):Ce3+,Tb3+荧光粉的发光性能优于传统高温固相法所制备的荧光粉。
(3)采用高温固相法制备了BaMgAl10O17:Eu2+(BAM:Eu2+)蓝色荧光粉。研究表明：合成工艺条件,诸如激活离子浓度、烧结温度和时间、还原温度和时间等,对BAM晶体结晶度、物相纯度、粉体颗粒形貌和发光强度有较大影响；少量Sr取代Ba对基质晶体结构的影响很小,Sr的掺入使BAM蓝粉的相对发光亮度下降,但可以提高其抗热劣化性能。采用实验所获得的较优条件所制备的Ba0.82Sr0.08MgAl10O17:Eu0.1蓝粉粒度为3.24gm,色坐标为x=0.0151、y=0.075(与商品粉的色坐标x=0.0145、y=0.072接近),发光亮度基本相当,相对亮度为商品粉的98.3%,抗热劣化性能优于商品粉,符合PDP用蓝色荧光粉的要求。
采用不同的助熔剂,均能制备出BAM:Eu2+发光材料,且样品的形貌更规整、颗粒大小更趋均一；Eu2+的掺入对基质晶体结构没有明显的影响；随着烧结时间的延长,样品结晶更趋完整、杂相减少,粉体发光强度随之提高；采用不同的助熔剂,合成反应的机理发生变化,所得样品的结晶完整性、杂相组成和含量、发光中心的分布、粉体粒径等性能产生相应变化,最终导致样品的发光性能发生改变,样品的特征发射峰强度随AlF3、H3BO3、 MgF2、Li2CO3、无助熔剂依次降低。
(4)以SrAl2O4:Eu,Dy为合成对象,考察了喷雾热解法合成稀土发光材料的可行性。实验结果表明：只要控制好工艺技术条件,喷雾热解法是一可取的合成稀土发光材料的方法；较之高温固相法,喷雾热解法能在较低的温度下制备具有分散性好、粒度小、粒径分布窄(2μm～5μm)、形貌规则(实心球形)、发光性能优良等优点的发光材料。
喷雾热解两段法制备的SrAl2O4:Eu,Dy发光材料的晶体结构与a-SrAl2O4磷石英晶体结构相同,掺杂Eu、Dy对晶体结构的影响很小。金属离子总浓度、热解温度和还原温度对产物的形貌、粒度分布、发光性能有较大影响。随着还原温度的升高,产物的发射主峰位置发生红移。
添加剂的使用能明显改善和修饰材料的形貌、增强材料的初始亮度、延长材料的余辉时间(柠檬酸的使用会缩短材料的余辉时间)。柠檬酸的加入有助于获得实心球形颗粒,乙醇除了良好的分散性,还能有效的增大颗粒的球形度,但无法获得实心颗粒,PEG能够起到分散剂和稳定剂的作用。当三种添加剂同时使用时可获得初始亮度高、余辉时间长、分散性好、粒度小、粒径分布窄(2μm～5μm)的实心球形颗粒。
Plasma flat panel display technology eliminates the geometric distortion of the picture, and offers brightness uniformity, high color purity, high contrast, and other advantages. Plasma flat panels (PDPs) is the most promising candidate for large size flat-panel information-display devices, is a very important development direction of HDTV. Fluorescent powders are one of the key factors which determine display quality. PDP phosphor is excited by147nm or172nm vuv light, therefore, it should have good thermal stability, high luminous efficiency, small powder particle size, and a narrow range of grain size distribution, high color purity, afterglow time is short and other properties. The performance of present commodities-PDP phosphor has many shortcomings:(l)red phosphor:color purity of (Y,Gd) BO3:Eu3+red phosphor is not high, and light-emitting efficiency of Y2O3:Eu3+is relatively low, and (2)blue phosphor: Eu2+activated BAM phosphor has poor stability, and its peak maximum also shift during various stages of panel fabrication and (3)green powder:the decay time of Zn2SiO4:Mn2+phosphor is somewhat longer for practical application.
Therefore,(La,Ce,Tb) BO3green phosphor, Ln (BO3,PO4):Ce3+,Tb3+green phosphor, BAM:Eu2+blue phosphor for PDP are synthesized by high temperature solid state reaction and modified high temperature solid state reaction. SEM, XRD, TG-DTA, luminescence spectra and other means were used to study the phosphor samples. The effect of flux on high temperature solid state reaction mechanism and the feasibility of the spray pyrolysis synthesis using to synthesize rare earth luminescent materials were studied. The studied conclusions came following:
(1) The phosphors of (La,Ce,Tb)BO3was synthesized by high temperature solid state reaction. X-ray diffractometry (XRD) patterns indicate that the Crystal Structure of (La,Ce,Tb)BO3and LaBO3is the same. The crystal structure has not been changed by Ce3+and Tb3+mixed into. Emission scanning electron microscopy (SEM) images show that the particle size of phosphors is more uniform, morphology is more rules, and granularity is about5μm. The content of TbBO3phase in (La,Ce,Tb)BO3increases with increasing of Tb content in (La,Ce,Tb)BO3. When Tb concentration reaches15%and above, the content of TbBO3phase in (La,Ce,Tb)BO3increases more rapidly. The luminescence properties of (La,Ce,Tb)BO3and the sensitization of Ce3+to Tb3+were studied. There are three peaks at around244,268and330nm in the excitation spectrum of Ce3+, and there are two peaks at365and380nm in the emission spectrum of Ce3+, respectively. All of them have the large overlap. The excitation peaks of Tb3+is230nm and its Maximum emission wavelength is541nm. Both the Tb3+characteristic emission and excitation peaks and the Ce3+characteristic emission and excitation peaks were observed in the emission and excitation spectrum of (La,Ce,Tb)BO3. Comparing the emission spectrum of (La,Tb)BO3with the excitation spectrum of (La,Ce)BO3, and find them having the large overlap, it inferred that there is remarkable energy transfer from Ce3+to Tb3+in it. When the concentration of Ce or Tb in (La,Ce,Tb)BO3is fixed, because of concentration self-quenching effect, the relative intensity of main emission peak (at541nm)increases firstly and then decreases with increasing of the concentration of Tb or Ce. At fixed ratio of Ce concentration to Tb concentration, the relative intensity of the main emission peak of (La,Ce,Tb)BO3is the highest when La concentration in (La,Ce,Tb)BO3reaches70%. The sample with better luminescence properties will be obtained in variety range of Ce concentration to Tb concentration at fixed La concentration of80%. When La concentration is80%and above, the relative intensity of the main emission peak of (La,Ce,Tb)BO3will be highest at Ce concentration to Tb concentration of3/1. Comparing commercial phosphor (La,Ce,Tb)PO4with experimental (La,Ce,Tb)BO3phosphor, experimental (La,Ce,Tb)BO3phosphor has a little red shift at489nm and its relative emission intensity was94.7%of the commercial phosphor (La,Ce,Tb)PO4. Therefore, it is inferred that (La,Ce,Tb)BO3would be a promising PDP green-emitting phosphor.
(2) Cerium-and terbium-doped lanthanum borophosphate [Ln(BO3,PO4):Ce3+, Tb3+] phosphor have been prepared by a single-step calcination using self-made BPO4as borophosphate sourse. Fine crystal structures are observed by XRD patterns. The excitation spectrum of Ln(BO3,PO4):Ce3+,Tb3+(Ln=Y, La, Gd) includes host sensitization band at120-175nm which is relative to the BO33-and PO43-groups, and several bands at175-300nm originated from4f→5d transition of Tb3+. The replacement of the host leads to changes of fluorescence Intensity ratios and CIE coordinate in emission spectrum. Among these phosphors, Gd(BO3,PO4):Ce3+,Tb3+phosphor shows best green fluorescence intensity ratio. The lifetime of the emission transition3D4→7F4of Tb3+is2.92ms, with a10%afterglow of6.7ms, which make it better than Zn2SiO4:Mn2+commercial phosphor for PDP.
(3) BaMgAl10O17:Eu2+phosphors were synthesized by high temperature solid-state reaction method. Using the X-ray powder diffraction, scanning electron microscopy and photoluminescence spectra, the effect of different fluxes, reaction time on such properties as crystals crystallinity, phase purity, particle morphology, luminescence intensity and thermally stability of the blue phosphor were investigated. The mechanism of synthesis of BaMgAl10O17:Eu2+with different fluxes was analyzed. The results show that synthesis conditions such as flux, concentration of doped ions, sintering temperature and time, reduction temperature and time have important influence on crystals crystallinity, phase purity, particle morphology, luminescence intensity and thermally stability of the blue phosphor. Incorporation of Sr has little influence on crystal structure of BAM matrix, it would cause the drop of initial relative brightness of phosphor's, but the thermally stability of BAM luminous phosphor would be improved. When flux is adopted, BaMgAl10O17:Eu2+phosphors with more regular morphology, uniform particle size and crystals crystallinity can be obtained at lower sintering temperature. Incorporation of Eu2+has less influence on crystal structure of BaMgAl10O17matrix. Along with the agglutination time's extension, the sample's crystallization becomes more completely, the content of impurity phase in it reduces and its luminous intensity increase. As different fluxes are used, the mechanism of synthesis of BaMgAl10O17:Eu2+will change. The performances of prepared sample such as crystallization integrity, phase purity, the luminescent center distribution have corresponding change with the change of the synthesis mechanism, thus the luminescent properties of the samples change correspondingly.
Comparing the experimental blue phosphor obtained at optimized conditions (Ba0.82Sr0.08MgAl10O17:Eu0.1) with the commodity powder BAM, relative emission intensity of the experimental blue phosphor is98.3%of the commercial phosphor BAM, its color coordinate is close to the commercial phosphor (experimental blue phosphor's color coordinate is x=0.0145, y=0.072, and the color coordinate of commercial phosphor is x=0.0145, y=0.072). The experimental blue phosphor has better thermally stability than that of the commercial phosphor. The granularity of it was3.24μm Therefore, it is expected that the experimental blue phosphor would be used for PDP blue phosphor.
(4) Through the synthesis of SrAl2O4:Eu,Dy, the feasibility of the spray pyrolysis synthesis using to synthesize rare earth luminescent materials was studied. Experimental results show that spray pyrolysis method is a desirable method of synthesis of rare earth luminescence materials as long as the technology conditions are optimized. Compared with the SrAl2O4:Eu,Dy prepared by solid state method, the SrAl2O4:Eu,Dy prepared by spray pyrolysis has more regular morphology (compact solid spherical particles), smaller particle size, narrower particle size distribution and more excellent luminescent properties, and the synthesis temperature can be significantly reduced.
The SrAl2O4:Eu,Dy prepared by spray pyrolysis belongs to the α-SrAl2O4phosphor crystal structure and small amount of Eu, Dy doped into the matrix has little effect on the crystal structure of SrAl2O4. The morphology, size distribution and luminous performances of the phosphors could be affected with synthesizing conditions, such as precursor concentration, sintering temperature, reduction temperature etc. As the reduction temperature rised, red shift of the main peak position in the emission spectrum occurs (move to longer wavelengths).
Additives caould obviously improve the morphology, reinforce the initial brightness, and enlarge the afterlow time (citric acid would shorten the afterlow time). Citric acid could help to obtain solid spherical particle. Ethanol was not only a good dispersant but also improved the sphericity of particle. Howerve, solid spherical particles couldn't be gotten in this condition. PEG played the role of dispersant and stabilizer. The solid spherical SrAl2O4:Eu,Dy particles with high initial brightness, long twilight time, good dispersion, small particle size and narrow particle size distribution (2μm～5μm) when these additives was used at the same time.
引文
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