特殊价态离子掺杂荧光体的发光特性研究
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摘要
特殊价态离子掺杂荧光体具有一些突出优点和特殊的光学性能，使得这些材料有望被用来帮助人类解决所面对的一些问题，如：全球能源危机、环境污染、战争与和平、信息与通讯、健康与医疗等。因此，人们对特殊价态离子掺杂荧光体材料的研究越来越感兴趣。
本文首先系统地介绍了特殊价态离子掺杂荧光体发展历史、优点、特殊的发光性能、应用领域以及相关研究进展。然后介绍我们研究和开发的一些特殊价态离子掺杂荧光体，并通过现代测试方法对材料的发光性能进行表征和分析，探讨了这些发光材料在不同领域中的可能应用，最后对其特性进行了总结和归纳。研究内容和结果主要包括以下几个方面：
1、在200~360℃的温度范围和无水无氧条件下，利用融盐（AlCl_3-NaCl）作为反应媒介，制备了一种超宽带近-中红外发光的Bi_5(AlCl_4)_3晶体。探讨了Bi_5(AlCl_4)_3晶体生长的最佳工艺条件。我们首次发现了Bi_5(AlCl_4)_3晶体的发光范围覆盖1000~3000nm，半高宽为~700nm，发光中心位于~1700nm的近-中红外发光；Bi_5(AlCl_4)_3晶体发光是由于Bi_5~(3+)团簇离子引起的。分析了Bi_5(AlCl_4)_3晶体发光的影响因素，并与铋掺杂玻璃材料进行发光性能比较。利用能级图对Bi_5(AlCl_4)_3晶体中Bi_5~(3+)团簇离子的发光机理进行了分析和探讨。这种含有Bi_5~(3+)团簇离子的Bi_5(AlCl_4)_3晶体在环境、激光、通讯、国防和医疗等领域具有广泛的应用前景。
2、Bi_5(AlCl_4)_3晶体制备条件较苛刻，需要在高温下反应，并且制备的Bi_5(AlCl_4)_3晶体很难从融盐媒介中分离出来。我们研究了合成条件比较温和和晶体可以从反应媒介分离出来的Bi_5(GaCl_4)_3晶体。在室温和无水无氧条件下，利用有机溶剂（如：苯等）作为反应媒介制备了具有超宽带近-中红外发光的Bi_5(GaCl_4)_3晶体。探讨了Bi_5(GaCl_4)_3晶体生长的最佳工艺条件。Bi_5(GaCl_4)_3晶体发光范围在1000~3000nm，发光中心位于~1835nm，半高宽为~800nm；通过时间分辨光谱证明了Bi_5~(3+)团簇离子是Bi_5(GaCl_4)_3晶体中单一的发光中心。分析了影响Bi_5(GaCl_4)_3晶体发光的因素，通过控制不同的实验反应条件和原料对Bi_5(GaCl_4)_3晶体中Bi_5~(3+)团簇离子的发光特性进行了探讨。这种含有Bi_5~(3+)团簇离子的Bi_5(GaCl_4)_3晶体在环境、激光、通讯、国防和医疗等领域具有广泛的应用前景。
3、在空气中和温度为650~750℃的实验条件下，利用融盐（KCl-NaCl）作为反应媒介制备了具有超宽带近红外发光的Mn离子掺杂的BaSO_4晶体。探讨了Mn离子掺杂的BaSO_4晶体生长的最佳工艺条件。Mn离子掺杂的BaSO_4晶体同时含有Mn~(5+)和Mn~(6+)离子。Mn~(5+)离子发光范围在1100~1400nm，发光中心位于~1183nm，半高宽为~50nm；Mn~(6+)离子发光范围在850~1500nm，发光中心位于~1060nm，半高宽为~150nm。分析了影响Mn离子掺杂的BaSO_4晶体发光的因素，时间分辨光谱证实了Mn离子掺杂的BaSO_4晶体中的Mn~(5+)和Mn~(6+)离子之间存在能量传递。通过温度和原料控制可以制备Mn~(6+)离子掺杂的BaSO_4晶体以及不同价态锰离子（如：Mn~(5+)和Mn~(6+)等）共同掺杂的BaSO_4晶体。Mn离子掺杂的BaSO_4晶体在激光和国防等领域中具有一定的应用前景。
4、在空气中采用高温固相法合成了BaSO_4:Bi~(2+)红色荧光粉。探讨了BaSO_4:Bi~(2+)红色荧光粉合成的最佳工艺条件。BaSO_4:Bi~(2+)红色荧光粉可以被~452nm蓝光激发产生发光中心位于~627nm的发射光，发射光谱覆盖范围为550~720nm，半高宽为~50nm。分析了影响BaSO_4:Bi~(2+)红色荧光粉发光的因素，证明了荧光粉中只有一个Bi~(2+)离子发光中心。利用环氧树脂+蓝光455nm发光二极管（LED）芯片+BaSO_4:Bi~(2+)红色荧光粉+Y_3Al_5O_(12):Ce~(3+0（YAG:Ce_(3+)）黄色荧光粉制备了白光LED，进行了白光LED发光演示和相应的光谱测试，白光LED的CIE色坐标为（x=0.3086，y=0.2902）、显色指数（Ra）为78和色温为7256K。实验结果表明，BaSO_4:Bi~(2+)红色荧光粉在蓝光LED芯片激发的白光LED中具有一定的应用前景。
5、采用高温固相法在空气中合成了Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉。探讨了Sr_2MgAl_(22)O_(36):Mn_(4+)红色荧光粉合成的最佳工艺条件。Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉可以被近紫外~397nm激发产生发光中心位于~658nm的发射光谱，发射光谱覆盖范围为620~750nm，半高宽为~50nm。分析了影响Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉发光的因素，证明了荧光粉中只有一个Mn~(4+)离子发光中心。利用环氧树脂+近紫外397nm LED芯片+Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉+(Sr, Ba)_2SiO_4:Eu~(2+)绿色荧光粉制备了白光LED，进行了白光LED发光演示和相应的光谱测试，白光LED的CIE色坐标为（x=0.3314，y=0.3211）、显色指数（Ra）为62.2和色温为5545K。实验结果表明，Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉在近紫外LED芯片激发的白光LED中具有一定的应用前景。
6、采用高温固相法在空气中合成了SrMgAl_x4+xO_(17±δ):yMn~(4+)复合红色荧光粉。探讨了(SrMgAlxO_(17)±δ:yMn~(4+)复合红色荧光粉合成的最佳条件。SrMgAlxO_(17)±δ:yMn~(4+)复合红色荧光粉可以被近紫外~397nm激发产生发光中心位于~657nm的发射光谱，发射光谱覆盖范围为620~750nm，半高宽为~50nm；SrMgAl_x4+xO_(17±δ):yMn~(4+)复合红色荧光粉中包含有含有SrMgAl10O17和Al_2O_3两种纯相，其中Al_2O_3纯相随Al含量增加越来越明显；发射光在Mn~(4+)离子掺杂的SrMgAl10O17和Al_2O_3两相之间可以产生多次吸收和散射，从而使得SrMgAl_x4+xO_(17±δ):yMn~(4+)复合红色荧光粉荧光强度增强；通过Al含量的变化可以制备不同荧光强度的红色荧光粉；荧光寿命和量子效率都随着Al含量的增加而增大；证明了荧光粉中只有一个Mn~(4+)离子发光中心；时间分辨光谱证实了SrMgAl_xO_(17)±δ:yMn~(4+)复合红色荧光粉中两个不同相之间存在能量传递现象。最后利用环氧树脂+近紫外397nmLED芯片+SrMgAl_xO_(17)±δ:yMn~(4+)复合红色荧光粉+(Sr, Ba)2SiO4:Eu2+绿色荧光粉制备了白光LED，进行发光演示和相应的光谱测试，白光LED的CIE色坐标为（x=0.3304，y=0.3201）、显色指数（Ra）为65.2和色温为5445K。实验结果表明，SrMgAl_xO_(17)±δ:yMn~(4+)复合红色荧光粉在近紫外LED芯片激发的白光LED中具有应用前景。
7、由于铋元素在掺杂材料中可以存在多种价态（如：Bi~(3+)、Bi~(2+)、Bi_2~(2+)、Bi~+、Bi0、Bi~(5+)和Bi3~(+5)等），有些价态在基质中的稳定性差，人们对于铋掺杂发光材料的发光机理（特别是近红外发光机理）还存在一些争议。本文主要是针对铋掺杂的氧化物玻璃中近-中红外发光机理进行分析和讨论。我们通过不同实验方法制备了Bi@SiO2、MF2:Bi（M=Ba和Sr）、MgF2:V和ZnS:Co材料，通过对这些材料的发光性能测试，发现这些材料在近-中红外发光区域具有和铋掺杂的氧化物玻璃（Bi_2O_3-GeO_2）相似的发光峰。经过分析，确认了铋掺杂的氧化物玻璃中中红外发光不是由铋离子引起的，推测其是由于空气在激光能量的激发下产生的热辐射造成的。这些研究结果对于铋掺杂发光材料的近-中红外发光机理研究有一定的指导意义。
8、在空气中采用高温固相法合成了RF_2:Bi（R=Ca和Sr）荧光粉。探讨了RF_2:Bi（R=Ca和Sr）荧光粉合成的最佳工艺条件。通过对RF_2:Bi（R=Ca和Sr）荧光粉的性能测试发现：在~260nm紫外光激发下，CaF2:Bi荧光粉在380~800nm范围内发射峰值位于~550nm的黄色光，SrF2:Bi荧光粉在400~810nm范围内发射峰值位于~600nm的橙色光。RF_2:Bi（R=Ca和Sr）荧光粉的发光可以确认为Bi~(2+)离子发光，其激发与发射峰分别归属于Bi~(2+)离子的~2P2221/2S1/2和P3/2(1) P1/2电子跃迁。这些研究结果对于铋掺杂发光材料的发光机理研究有一定的指导意义。
最后，对本文的重点进行了讨论和总结，并对特殊价态离子掺杂的荧光体发光性能和应用前景进行了展望。
Due to special performance of phosphors doped with special valence state ions, thesephosphors are promising to be used to resolve some problems in the human society, such asglobal energy crisis, environmental pollution, war and peace, information and communication,health and medical treatment etc. Therefore, researchers are interested in the study onphosphors doped with special valence state ions in recent years.
In this dissertation, we introduced the research developments on phosphors doped withspecial valence state ions, their luminescence properties, special performance and applicationsat first. Then we introduced the preparation of phosphors doped with special valence stateions, studied their luminescence properties via modern analysis techniques and discussed theirapplications in different fields. The research results in the dissertation can be summarized asfollow:
(1) Bi_5(AlCl_4)_3crystal was prepared in the200~360℃region under anhydrousanaerobic conditions using melting salt (AlCl_3-NaCl) as reaction media. Optimum synthesisconditions of Bi_5(AlCl_4)_3crystal were investigated. Broadband near-to-mid infrared(NIR-MIR) photoluminescence centering at~1700nm with full width at half maximum(FWHM)~700nm at room temperature, in the range of1000~3000nm was observed fromBi_5(AlCl_4)_3crystal due to a single type of Bi_5~(3+)luminescent center in Bi_5(AlCl_4)_3crystal. Wehave investigated the influencing factor of luminescence of Bi_5(AlCl_4)_3crystal, compared theluminescence properties with these of the glasses doped with Bi ion, and discussed theluminous mechanism of Bi_5~(3+)in Bi_5(AlCl_4)_3crystal based on the configurational coordinationdiagram. Bi_5(AlCl_4)_3crystal may have application in environment, laser, communication,national defense and medical treatment fields.
(2) Due to rigorous experiment conditions for preparation of Bi_5(AlCl_4)_3crystal such ashigh temperature etc, Bi_5(GaCl_4)_3crystal was prepared at room temperature under anhydrousanaerobic conditions using organic solvent (such as benzene etc) as reaction media. Optimumsynthesis conditions of Bi_5(GaCl_4)_3crystal were investigated. Superbroad NIR-MIRphotoluminescence centering at~1835nm with full width at half maximum (FWHM)~800nm at room temperature, in the range of1000to3000nm was observed from Bi_5(GaCl_4)_3crystal due to a single type of Bi_5~(3+)luminescence center in Bi_5(GaCl_4)_3crystal. We haveinvestigated the influencing factors of luminescence of Bi_5(GaCl_4)_3crystal and discussed theluminous mechanism of Bi_5~(3+)in Bi_5(GaCl_4)_3crystal. Bi_5(GaCl_4)_3crystal may have applicationin environment, laser, communication, national defense and medical treatment fields.
(3) Mn ions-doped BaSO_4crystal was prepared in the650~750℃region in air usingmelting salt (KCl-NaCl) as reaction media. Broadband near infrared (NIR) luminescence wasobserved. Optimum synthesis conditions of Mn ions-doped BaSO_4crystal were investigated.The concomitant Mn~(5+)and Mn~(6+)ions in the Mn ions-doped BaSO_4crystal were confirmed.NIR luminescence was observed from Mn~(5+)ion in Mn ions-doped BaSO_4crystal centering at~1183nm with full width at half maximum (FWHM)~50nm at room temperature, spanningthe spectral range of1100to1400nm. NIR luminescence was observed from Mn~(6+)ion in Mnions-doped BaSO_4crystal centering at~1060nm with FWHM of~150nm at roomtemperature, in the range of850to1500nm. We have investigated the influencing factor ofluminescence of Mn ions-doped BaSO_4crystal and observed the energy transfer betweenMn~(5+)and Mn~(6+)ions in Mn ions-doped BaSO_4crystal according to time resolvedluminescence spectra. In addition, Mn~(6+)ion-doped BaSO_4crystal was also prepared. Mnions-doped BaSO_4crystal may have application in laser and national defense fields.
(4) BaSO_4:Bi~(2+)red emission phosphor was synthesized in air via solid state reactionmethod. Optimum synthesis conditions of BaSO_4:Bi~(2+)phosphors were investigated. Theemission band peaking at~627nm in the range of550to720nm with FWHM of~50nm ofBaSO_4:Bi~(2+)excited at452nm was observed at room temperature. We have investigated theinfluencing factor of luminescence of BaSO_4:Bi~(2+)phosphor and confirmed that Bi~(2+)ion isonly luminescent center. White light-emitting diode (W-LED) was fabricated by using epoxyresin, a blend composition BaSO_4:Bi~(2+)and Y3Al5O12:Ce3+(YAG:Ce3+) phosphors pumpedwith a455nm blue LED chip. The white LED shows chromaticity coordinates (x=0.3086，y=0.2902), Ra value78and CCT (7256K). BaSO_4:Bi~(2+)red emission phosphor may haveapplication in W-LED fields.
(5) Sr_2MgAl_(22)O_(36):Mn~(4+)red emission phosphor was synthesized in air via solid statereaction method. Optimum synthesis conditions of Sr42MgAl22O36:Mn+phosphors wereinvestigated. The emission band peaking at~658nm in the range of620to750nm withFWHM is~50nm of Sr4+2MgAl22O36:Mnexcited at397nm was observed at roomtemperature. We have investigated the influencing factor of luminescence ofSr_2MgAl_(22)O_(36):Mn~(4+)phosphor and confirmed that Mn~(4+)ion is only luminescent center. Whitelight-emitting diode (W-LED) was fabricated by using epoxy resin, a blend compositionSr_2MgAl_(22)O_(36):Mn~(4+)and (Sr, Ba)22SiO4:Eu+phosphors pumped with a397nm near ultraviolet(UV) LED chip. The white LED shows chromaticity coordinates (x=0.3314，y=0.3211), Ravalue62.2and CCT (5545K). Sr_2MgAl_(22)O_(36):Mn~(4+)red emission phosphor may have application in W-LED fields.
(6) SrMgAl_4+xO_(17)±δ: yMnred emission composite phosphor was synthesized in air viasolid state reaction method. Optimum synthesis conditions of SrMgAl_x4+xO_(17±δ):yMn~(4+)compositephosphors were investigated. The emission band peaking at~657nm in the range of620to750nm with FWHM of~50nm of SrMgAl_xO_(17)±δ: yMn~(4+)excited at397nm was observed atroom temperature. Two concomitant crystalline phases, i.e., SrMaAl10O17and Al_2O_3phases inSrMgAl4xO17±δ:yMn+composite phosphors were observed. Energy transfer was observedbetween Mn~(4+)-doped in SrMgAl4+10O17and Mn-doped in Al_2O_3phases by using time resolvedluminescence spectra. The emission intensity of SrMgAl_xO_(17)±δ:yMn~(4+)composite phosphorchanged with changing Al_2O_3content, and confirmed that Mn~(4+)ion is only luminescent center.Fluorescent lifetime and quantum efficiency increased with increasing Al_2O_3content.W-LEDs were demonstrated by using epoxy resin, a phosphors blend compositionSrMgAl_xO_(17)±δ:1.2Mn~(4+)and (Sr, Ba)2SiO_4:Eu2+phosphors pumped with a397nm nearUV-chip. The white LED shows chromaticity coordinates (x=0.3304，y=0.3201), Ra value65.2and CCT (5445K). SrMgAl_xO_(17)±δ: yMn~(4+)composite phosphor may have application inW-LED fields.
(7) Optically active emission centers in Bi-doped luminescent materials, especially forNIR emission, remains disputed due to the large number of possible valence states such asBi3+, Bi~(2+), Bi~(2+)02, Bi~+, Bi, Bi~(5+)and Bi_5~(3+)etc and weak stability of Bi valence states in varioushosts. We disscussed the optically active NIR emission centers in Bi-doped oxide glasses. Weprepared Bi@SiO_2, MF_2:Bi (M=Ba and Sr), MgF_2:V and ZnS:Co via various methods, andfound some emission band in the mid luminescence region with Bi-doped Bi2O3-GeO2glassreported by jiang et al. We concluded that the emission is not result from Bi active centers inthe oxide matrix but due to the selective atmospheric absorption of thermal radiation inducedby the laser irradiation. The research result is helpful for clarifying the optically active NIRemission center in Bi-doped luminescent materials..
(8) RF_2:Bi（R=Ca and Sr）phosphor was synthesized in air via solid state reactionmethod. Optimum synthesis conditions of RF_2:B（iR=Ca and Sr）phosphor were investigated.The emission band peaking at~550nm in the range of380to800nm of CaF2:Bi phosphorexcited at~260nm was observed, and the emission band peaking at~600nm in the range of400to810nm of SrF2:Bi phosphor excited at~260nm was observed. Optically activeemission centers in RF_2:Bi（R=Ca and Sr）phosphor is Bi~(2+)and the excitation and emissionbands of RF_2:B（iR=Ca and Sr）phosphor can be assigned to2P221/2S1/2andP3/2(1)2P1/2 transition of Bi~(2+)ions, respectively. The research results are of reference value for disigningin Bi-doped luminescent materials.
Finally, we provided a discussion and summary of the main points of the dissertation,and described the application prospect of phosphors doped with special valence state ions invarious fields.
本文首先系统地介绍了特殊价态离子掺杂荧光体发展历史、优点、特殊的发光性能、应用领域以及相关研究进展。然后介绍我们研究和开发的一些特殊价态离子掺杂荧光体，并通过现代测试方法对材料的发光性能进行表征和分析，探讨了这些发光材料在不同领域中的可能应用，最后对其特性进行了总结和归纳。研究内容和结果主要包括以下几个方面：
1、在200~360℃的温度范围和无水无氧条件下，利用融盐（AlCl_3-NaCl）作为反应媒介，制备了一种超宽带近-中红外发光的Bi_5(AlCl_4)_3晶体。探讨了Bi_5(AlCl_4)_3晶体生长的最佳工艺条件。我们首次发现了Bi_5(AlCl_4)_3晶体的发光范围覆盖1000~3000nm，半高宽为~700nm，发光中心位于~1700nm的近-中红外发光；Bi_5(AlCl_4)_3晶体发光是由于Bi_5~(3+)团簇离子引起的。分析了Bi_5(AlCl_4)_3晶体发光的影响因素，并与铋掺杂玻璃材料进行发光性能比较。利用能级图对Bi_5(AlCl_4)_3晶体中Bi_5~(3+)团簇离子的发光机理进行了分析和探讨。这种含有Bi_5~(3+)团簇离子的Bi_5(AlCl_4)_3晶体在环境、激光、通讯、国防和医疗等领域具有广泛的应用前景。
2、Bi_5(AlCl_4)_3晶体制备条件较苛刻，需要在高温下反应，并且制备的Bi_5(AlCl_4)_3晶体很难从融盐媒介中分离出来。我们研究了合成条件比较温和和晶体可以从反应媒介分离出来的Bi_5(GaCl_4)_3晶体。在室温和无水无氧条件下，利用有机溶剂（如：苯等）作为反应媒介制备了具有超宽带近-中红外发光的Bi_5(GaCl_4)_3晶体。探讨了Bi_5(GaCl_4)_3晶体生长的最佳工艺条件。Bi_5(GaCl_4)_3晶体发光范围在1000~3000nm，发光中心位于~1835nm，半高宽为~800nm；通过时间分辨光谱证明了Bi_5~(3+)团簇离子是Bi_5(GaCl_4)_3晶体中单一的发光中心。分析了影响Bi_5(GaCl_4)_3晶体发光的因素，通过控制不同的实验反应条件和原料对Bi_5(GaCl_4)_3晶体中Bi_5~(3+)团簇离子的发光特性进行了探讨。这种含有Bi_5~(3+)团簇离子的Bi_5(GaCl_4)_3晶体在环境、激光、通讯、国防和医疗等领域具有广泛的应用前景。
3、在空气中和温度为650~750℃的实验条件下，利用融盐（KCl-NaCl）作为反应媒介制备了具有超宽带近红外发光的Mn离子掺杂的BaSO_4晶体。探讨了Mn离子掺杂的BaSO_4晶体生长的最佳工艺条件。Mn离子掺杂的BaSO_4晶体同时含有Mn~(5+)和Mn~(6+)离子。Mn~(5+)离子发光范围在1100~1400nm，发光中心位于~1183nm，半高宽为~50nm；Mn~(6+)离子发光范围在850~1500nm，发光中心位于~1060nm，半高宽为~150nm。分析了影响Mn离子掺杂的BaSO_4晶体发光的因素，时间分辨光谱证实了Mn离子掺杂的BaSO_4晶体中的Mn~(5+)和Mn~(6+)离子之间存在能量传递。通过温度和原料控制可以制备Mn~(6+)离子掺杂的BaSO_4晶体以及不同价态锰离子（如：Mn~(5+)和Mn~(6+)等）共同掺杂的BaSO_4晶体。Mn离子掺杂的BaSO_4晶体在激光和国防等领域中具有一定的应用前景。
4、在空气中采用高温固相法合成了BaSO_4:Bi~(2+)红色荧光粉。探讨了BaSO_4:Bi~(2+)红色荧光粉合成的最佳工艺条件。BaSO_4:Bi~(2+)红色荧光粉可以被~452nm蓝光激发产生发光中心位于~627nm的发射光，发射光谱覆盖范围为550~720nm，半高宽为~50nm。分析了影响BaSO_4:Bi~(2+)红色荧光粉发光的因素，证明了荧光粉中只有一个Bi~(2+)离子发光中心。利用环氧树脂+蓝光455nm发光二极管（LED）芯片+BaSO_4:Bi~(2+)红色荧光粉+Y_3Al_5O_(12):Ce~(3+0（YAG:Ce_(3+)）黄色荧光粉制备了白光LED，进行了白光LED发光演示和相应的光谱测试，白光LED的CIE色坐标为（x=0.3086，y=0.2902）、显色指数（Ra）为78和色温为7256K。实验结果表明，BaSO_4:Bi~(2+)红色荧光粉在蓝光LED芯片激发的白光LED中具有一定的应用前景。
5、采用高温固相法在空气中合成了Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉。探讨了Sr_2MgAl_(22)O_(36):Mn_(4+)红色荧光粉合成的最佳工艺条件。Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉可以被近紫外~397nm激发产生发光中心位于~658nm的发射光谱，发射光谱覆盖范围为620~750nm，半高宽为~50nm。分析了影响Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉发光的因素，证明了荧光粉中只有一个Mn~(4+)离子发光中心。利用环氧树脂+近紫外397nm LED芯片+Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉+(Sr, Ba)_2SiO_4:Eu~(2+)绿色荧光粉制备了白光LED，进行了白光LED发光演示和相应的光谱测试，白光LED的CIE色坐标为（x=0.3314，y=0.3211）、显色指数（Ra）为62.2和色温为5545K。实验结果表明，Sr_2MgAl_(22)O_(36):Mn~(4+)红色荧光粉在近紫外LED芯片激发的白光LED中具有一定的应用前景。
6、采用高温固相法在空气中合成了SrMgAl_x4+xO_(17±δ):yMn~(4+)复合红色荧光粉。探讨了(SrMgAlxO_(17)±δ:yMn~(4+)复合红色荧光粉合成的最佳条件。SrMgAlxO_(17)±δ:yMn~(4+)复合红色荧光粉可以被近紫外~397nm激发产生发光中心位于~657nm的发射光谱，发射光谱覆盖范围为620~750nm，半高宽为~50nm；SrMgAl_x4+xO_(17±δ):yMn~(4+)复合红色荧光粉中包含有含有SrMgAl10O17和Al_2O_3两种纯相，其中Al_2O_3纯相随Al含量增加越来越明显；发射光在Mn~(4+)离子掺杂的SrMgAl10O17和Al_2O_3两相之间可以产生多次吸收和散射，从而使得SrMgAl_x4+xO_(17±δ):yMn~(4+)复合红色荧光粉荧光强度增强；通过Al含量的变化可以制备不同荧光强度的红色荧光粉；荧光寿命和量子效率都随着Al含量的增加而增大；证明了荧光粉中只有一个Mn~(4+)离子发光中心；时间分辨光谱证实了SrMgAl_xO_(17)±δ:yMn~(4+)复合红色荧光粉中两个不同相之间存在能量传递现象。最后利用环氧树脂+近紫外397nmLED芯片+SrMgAl_xO_(17)±δ:yMn~(4+)复合红色荧光粉+(Sr, Ba)2SiO4:Eu2+绿色荧光粉制备了白光LED，进行发光演示和相应的光谱测试，白光LED的CIE色坐标为（x=0.3304，y=0.3201）、显色指数（Ra）为65.2和色温为5445K。实验结果表明，SrMgAl_xO_(17)±δ:yMn~(4+)复合红色荧光粉在近紫外LED芯片激发的白光LED中具有应用前景。
7、由于铋元素在掺杂材料中可以存在多种价态（如：Bi~(3+)、Bi~(2+)、Bi_2~(2+)、Bi~+、Bi0、Bi~(5+)和Bi3~(+5)等），有些价态在基质中的稳定性差，人们对于铋掺杂发光材料的发光机理（特别是近红外发光机理）还存在一些争议。本文主要是针对铋掺杂的氧化物玻璃中近-中红外发光机理进行分析和讨论。我们通过不同实验方法制备了Bi@SiO2、MF2:Bi（M=Ba和Sr）、MgF2:V和ZnS:Co材料，通过对这些材料的发光性能测试，发现这些材料在近-中红外发光区域具有和铋掺杂的氧化物玻璃（Bi_2O_3-GeO_2）相似的发光峰。经过分析，确认了铋掺杂的氧化物玻璃中中红外发光不是由铋离子引起的，推测其是由于空气在激光能量的激发下产生的热辐射造成的。这些研究结果对于铋掺杂发光材料的近-中红外发光机理研究有一定的指导意义。
8、在空气中采用高温固相法合成了RF_2:Bi（R=Ca和Sr）荧光粉。探讨了RF_2:Bi（R=Ca和Sr）荧光粉合成的最佳工艺条件。通过对RF_2:Bi（R=Ca和Sr）荧光粉的性能测试发现：在~260nm紫外光激发下，CaF2:Bi荧光粉在380~800nm范围内发射峰值位于~550nm的黄色光，SrF2:Bi荧光粉在400~810nm范围内发射峰值位于~600nm的橙色光。RF_2:Bi（R=Ca和Sr）荧光粉的发光可以确认为Bi~(2+)离子发光，其激发与发射峰分别归属于Bi~(2+)离子的~2P2221/2S1/2和P3/2(1) P1/2电子跃迁。这些研究结果对于铋掺杂发光材料的发光机理研究有一定的指导意义。
最后，对本文的重点进行了讨论和总结，并对特殊价态离子掺杂的荧光体发光性能和应用前景进行了展望。
Due to special performance of phosphors doped with special valence state ions, thesephosphors are promising to be used to resolve some problems in the human society, such asglobal energy crisis, environmental pollution, war and peace, information and communication,health and medical treatment etc. Therefore, researchers are interested in the study onphosphors doped with special valence state ions in recent years.
In this dissertation, we introduced the research developments on phosphors doped withspecial valence state ions, their luminescence properties, special performance and applicationsat first. Then we introduced the preparation of phosphors doped with special valence stateions, studied their luminescence properties via modern analysis techniques and discussed theirapplications in different fields. The research results in the dissertation can be summarized asfollow:
(1) Bi_5(AlCl_4)_3crystal was prepared in the200~360℃region under anhydrousanaerobic conditions using melting salt (AlCl_3-NaCl) as reaction media. Optimum synthesisconditions of Bi_5(AlCl_4)_3crystal were investigated. Broadband near-to-mid infrared(NIR-MIR) photoluminescence centering at~1700nm with full width at half maximum(FWHM)~700nm at room temperature, in the range of1000~3000nm was observed fromBi_5(AlCl_4)_3crystal due to a single type of Bi_5~(3+)luminescent center in Bi_5(AlCl_4)_3crystal. Wehave investigated the influencing factor of luminescence of Bi_5(AlCl_4)_3crystal, compared theluminescence properties with these of the glasses doped with Bi ion, and discussed theluminous mechanism of Bi_5~(3+)in Bi_5(AlCl_4)_3crystal based on the configurational coordinationdiagram. Bi_5(AlCl_4)_3crystal may have application in environment, laser, communication,national defense and medical treatment fields.
(2) Due to rigorous experiment conditions for preparation of Bi_5(AlCl_4)_3crystal such ashigh temperature etc, Bi_5(GaCl_4)_3crystal was prepared at room temperature under anhydrousanaerobic conditions using organic solvent (such as benzene etc) as reaction media. Optimumsynthesis conditions of Bi_5(GaCl_4)_3crystal were investigated. Superbroad NIR-MIRphotoluminescence centering at~1835nm with full width at half maximum (FWHM)~800nm at room temperature, in the range of1000to3000nm was observed from Bi_5(GaCl_4)_3crystal due to a single type of Bi_5~(3+)luminescence center in Bi_5(GaCl_4)_3crystal. We haveinvestigated the influencing factors of luminescence of Bi_5(GaCl_4)_3crystal and discussed theluminous mechanism of Bi_5~(3+)in Bi_5(GaCl_4)_3crystal. Bi_5(GaCl_4)_3crystal may have applicationin environment, laser, communication, national defense and medical treatment fields.
(3) Mn ions-doped BaSO_4crystal was prepared in the650~750℃region in air usingmelting salt (KCl-NaCl) as reaction media. Broadband near infrared (NIR) luminescence wasobserved. Optimum synthesis conditions of Mn ions-doped BaSO_4crystal were investigated.The concomitant Mn~(5+)and Mn~(6+)ions in the Mn ions-doped BaSO_4crystal were confirmed.NIR luminescence was observed from Mn~(5+)ion in Mn ions-doped BaSO_4crystal centering at~1183nm with full width at half maximum (FWHM)~50nm at room temperature, spanningthe spectral range of1100to1400nm. NIR luminescence was observed from Mn~(6+)ion in Mnions-doped BaSO_4crystal centering at~1060nm with FWHM of~150nm at roomtemperature, in the range of850to1500nm. We have investigated the influencing factor ofluminescence of Mn ions-doped BaSO_4crystal and observed the energy transfer betweenMn~(5+)and Mn~(6+)ions in Mn ions-doped BaSO_4crystal according to time resolvedluminescence spectra. In addition, Mn~(6+)ion-doped BaSO_4crystal was also prepared. Mnions-doped BaSO_4crystal may have application in laser and national defense fields.
(4) BaSO_4:Bi~(2+)red emission phosphor was synthesized in air via solid state reactionmethod. Optimum synthesis conditions of BaSO_4:Bi~(2+)phosphors were investigated. Theemission band peaking at~627nm in the range of550to720nm with FWHM of~50nm ofBaSO_4:Bi~(2+)excited at452nm was observed at room temperature. We have investigated theinfluencing factor of luminescence of BaSO_4:Bi~(2+)phosphor and confirmed that Bi~(2+)ion isonly luminescent center. White light-emitting diode (W-LED) was fabricated by using epoxyresin, a blend composition BaSO_4:Bi~(2+)and Y3Al5O12:Ce3+(YAG:Ce3+) phosphors pumpedwith a455nm blue LED chip. The white LED shows chromaticity coordinates (x=0.3086，y=0.2902), Ra value78and CCT (7256K). BaSO_4:Bi~(2+)red emission phosphor may haveapplication in W-LED fields.
(5) Sr_2MgAl_(22)O_(36):Mn~(4+)red emission phosphor was synthesized in air via solid statereaction method. Optimum synthesis conditions of Sr42MgAl22O36:Mn+phosphors wereinvestigated. The emission band peaking at~658nm in the range of620to750nm withFWHM is~50nm of Sr4+2MgAl22O36:Mnexcited at397nm was observed at roomtemperature. We have investigated the influencing factor of luminescence ofSr_2MgAl_(22)O_(36):Mn~(4+)phosphor and confirmed that Mn~(4+)ion is only luminescent center. Whitelight-emitting diode (W-LED) was fabricated by using epoxy resin, a blend compositionSr_2MgAl_(22)O_(36):Mn~(4+)and (Sr, Ba)22SiO4:Eu+phosphors pumped with a397nm near ultraviolet(UV) LED chip. The white LED shows chromaticity coordinates (x=0.3314，y=0.3211), Ravalue62.2and CCT (5545K). Sr_2MgAl_(22)O_(36):Mn~(4+)red emission phosphor may have application in W-LED fields.
(6) SrMgAl_4+xO_(17)±δ: yMnred emission composite phosphor was synthesized in air viasolid state reaction method. Optimum synthesis conditions of SrMgAl_x4+xO_(17±δ):yMn~(4+)compositephosphors were investigated. The emission band peaking at~657nm in the range of620to750nm with FWHM of~50nm of SrMgAl_xO_(17)±δ: yMn~(4+)excited at397nm was observed atroom temperature. Two concomitant crystalline phases, i.e., SrMaAl10O17and Al_2O_3phases inSrMgAl4xO17±δ:yMn+composite phosphors were observed. Energy transfer was observedbetween Mn~(4+)-doped in SrMgAl4+10O17and Mn-doped in Al_2O_3phases by using time resolvedluminescence spectra. The emission intensity of SrMgAl_xO_(17)±δ:yMn~(4+)composite phosphorchanged with changing Al_2O_3content, and confirmed that Mn~(4+)ion is only luminescent center.Fluorescent lifetime and quantum efficiency increased with increasing Al_2O_3content.W-LEDs were demonstrated by using epoxy resin, a phosphors blend compositionSrMgAl_xO_(17)±δ:1.2Mn~(4+)and (Sr, Ba)2SiO_4:Eu2+phosphors pumped with a397nm nearUV-chip. The white LED shows chromaticity coordinates (x=0.3304，y=0.3201), Ra value65.2and CCT (5445K). SrMgAl_xO_(17)±δ: yMn~(4+)composite phosphor may have application inW-LED fields.
(7) Optically active emission centers in Bi-doped luminescent materials, especially forNIR emission, remains disputed due to the large number of possible valence states such asBi3+, Bi~(2+), Bi~(2+)02, Bi~+, Bi, Bi~(5+)and Bi_5~(3+)etc and weak stability of Bi valence states in varioushosts. We disscussed the optically active NIR emission centers in Bi-doped oxide glasses. Weprepared Bi@SiO_2, MF_2:Bi (M=Ba and Sr), MgF_2:V and ZnS:Co via various methods, andfound some emission band in the mid luminescence region with Bi-doped Bi2O3-GeO2glassreported by jiang et al. We concluded that the emission is not result from Bi active centers inthe oxide matrix but due to the selective atmospheric absorption of thermal radiation inducedby the laser irradiation. The research result is helpful for clarifying the optically active NIRemission center in Bi-doped luminescent materials..
(8) RF_2:Bi（R=Ca and Sr）phosphor was synthesized in air via solid state reactionmethod. Optimum synthesis conditions of RF_2:B（iR=Ca and Sr）phosphor were investigated.The emission band peaking at~550nm in the range of380to800nm of CaF2:Bi phosphorexcited at~260nm was observed, and the emission band peaking at~600nm in the range of400to810nm of SrF2:Bi phosphor excited at~260nm was observed. Optically activeemission centers in RF_2:Bi（R=Ca and Sr）phosphor is Bi~(2+)and the excitation and emissionbands of RF_2:B（iR=Ca and Sr）phosphor can be assigned to2P221/2S1/2andP3/2(1)2P1/2 transition of Bi~(2+)ions, respectively. The research results are of reference value for disigningin Bi-doped luminescent materials.
Finally, we provided a discussion and summary of the main points of the dissertation,and described the application prospect of phosphors doped with special valence state ions invarious fields.
引文
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