氧化铝基发光材料的研究
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摘要
本文在国内外综合研究发光材料的发展历程、发光材料的定义、发光材料的组成、发光材料的分类、发光机理、性能表征、制备方法及其应用等基础上，分析了当前国内外发光材料的研究状况和所存在的问题。选取氧化铝基红色荧光粉作为研究重点，以求降低商业红粉的价格，改善其性能。
以硝酸铝为主要原料，用碳酸氢铵和氨水作为混合沉淀剂，采用反向滴定共沉淀工艺制备荧光粉体，并对其性能进行研究。研究内容和主要结论如下：
(1)用反向滴定共沉淀工艺制备氧化铝前驱体碳酸铝铵，并对制备工艺进行优化。研究表明：当金属铝盐溶液浓度控制在0.2mol／L，pH值为3～4之间：混合沉淀剂溶液浓度为2mol／L，pH值控制在9～10之间。碳酸氢铵与金属铝盐摩尔比为10，采用反向滴定缓慢(小于0.8L／h)加入的方法，可以得到团聚较少、物相单一、性能优良的前驱体碳酸铝铵。
(2)在不同温度下煅烧前驱体碳酸铝铵，利用TG-DSC，XRD研究其相变过程，得到碳酸铝铵的相变过程为：碳酸铝铵→非晶态氧化铝→γ→氧化铝→θ-氧化铝→α-氧化铝。通过激发光谱和发射光谱分析得到：监测波长为395nm时，氧化铝基体的激发光谱是以247nm为中心220nm到270nm的宽带激发；用254nm波长激发的发射光谱，是以395nm为中心340nm到460nm的宽带发射，发光峰位并不随着煅烧温度的变化而发生变化。而发光强度却有很大的变化，这是内部两种不同作用机制对F~+色心(氧空穴)发光的影响造成的。随着激发波长的增大，发射光谱的主峰位有了一定红移。
(3)制备了Al_2O_3：Eu和Al_2O_3：Eu、Tb发光粉体，利用TG-DSC，XRD，SEM和荧光分光光度计对其相变和发光特性进行研究，得出：稀土Eu、Tb的加入对氧化铝的相变有很大抑制作用，增强了γ-Al_2O_3的热稳定性，掺杂量越多对氧化铝的相变及结晶过程影响越大。Al_2O_3：Eu发光粉体，在掺杂量为1mol％，煅烧温度为1050℃，煅烧时间为4h时，得到发光强度最大的红色荧光粉。通过实验和分析，粉体的主要发射峰(614nm)是Eu~(3+)离子~5D_0-~7F_2能级的跃迁。Tb的掺入，提高了其发光强度，最佳掺杂量为5mol％。
(4)制备和研究了GdAlO_3：Eu和(Gd，Y)AlO_3：Eu发光粉体，利用TG-DSC，XRD和荧光分光光度计对其相变和发光特性进行研究，得出：1200℃煅烧2h即可得到物相单一，发光强度良好的荧光粉体。在Eu掺杂量为3mol％时，GdAlO_3：Eu发光粉体的主要发射峰609nm(~5D_0→~7F_2)强度最大。随着煅烧温度的升高，发射强度增大，到1200℃最大。用Y~(3+)替代部分Gd~(3+)离子时，从发射光谱图表现来看，越是趋向于单一的GdAlO_3或者YAlO_3相时，发光强度越大。它们是很好的红粉Y_2O_3：Eu的替代产品。
最后，对进一步的研究工作和研究方向作了展望。
At the beginning ,according to the basic knowledge about phylogeny , definition , makeup , sorts , luminescent mechanism , preparing methods and applications of luminescence materials ,current research information and subsistent problems of luminescence materials at home and abroad were analyzed in this paper . Red fluorescence powders that use alumina as the matrix were regarded as our research emphases in order to reduce the price of red powders commercially and improve its performances .Research contents and results are as follows:
Fluorescence powders were prepared by using Al(NO_3)-3·9H_2O as the main raw material and using NH_4HCO_3 and urea as the mixed precipitator to adoptthe reverse titration co-precipitation technology . Its performances were studied. The paper consists of four main parts .
Firstly , the precursor NH_4AlO(OH)HCO_3 was prepared by this method that has been optimized. The study about preparing the precursor NH_4AlO(OH)HCO_3(indicates : when the concentration and the pH value of Al(NO_3)_3 solution are 0.2mol/L and 3～4 respectively ;when the concentration and the pH value of the mixed precipitator are 2mol/L and 9～10 respectively ;when the molar ratio of NH_4HCO_3 and Al(NO_3)_3 is 10 , the well dispersive , single phase and excellent performance precursor NH_4AlO(OH)HCO_3 can be obtained by the reverse slow titration (less than 0. 8L/h).
Secondly ,the phase change of powders that were obtained by calcining the precursor NH_4AlO(OH)HCO_3 at different temperatures was studied through TG-DSC and XRD . The process of phase change is that : NH_4AlO(OH)HCO_3→amorphous alumina→γ-alumina→θ-alumina→α-alumina . Through excitation spectra and emission spectra of powders , we get that : When detected at wavelength 395nm ,excitation spectra of alumina matrix is a broad band from 220nm to 270nm at the center of 247nm . Under 254nm excitation, emission spectra of alumina matrix is also a broad band from 340nm to 460nm at the center of 395nm .When the calcining temperatures change ,the location of the peak does not change ,but the intensity changes strongly . The reason is that the luminescence intensity of F~+ color center is effected by the two different mechanisms .When the excitation wavelength becomes bigger , the main peak of emission spectra has some red shift.
Thirdly , the luminescence powders of Al_2O_3: Eu and Al_2O_3:Eu、Tb were prepared . Through TG-DSC, XRD, SEM and fluorescence spectrophotometer, their phases and luminescence property were studied .The results are that :When adding the rare earths of Eu or Tb , the phase change is greatly restrained and the thermal stability ofγ-Al_2O_3 becomes stronger . Adding quantity is more , the effects to the phase change and the crystallization process of alumina are bigger .When the Al_2O_3:Eu powder is calcined at 1050℃for 4h and concentration of Eu~(3+) dopant is 1mol% , Red fluorescence powder Al_2O_3:Eu that has the strongest luminescence intensity is obtained .Through experiments and analysis , the main peak at 614nm is the ~5D_0- ~7F_2 transition of Eu~(3+) ions . Adding Tb can improve the luminescence intensity of Al_2O_3: Eu powder. The optimum concentration of Tb~(3+) dopant is 5mol% .
Fourthly , the luminescence powders of GdAlO_3:Eu and (Gd,Y)AlO_3:Eu were prepared and studied . Through TG-DSC, XRD and fluorescence spectrophotometer, their phases and luminescence property were studied . The results are that : The GdAlO_3:Eu powder calcined at 1200℃for 2h has high luminescence intensity and pure phase . When optimum concentration of Eu~(3+) dopant is 3mol%, the main emission peak is at 609nm (~5D_0→~7F_2) under 254nm excitation .With the calcining temperature increasing ,the luminescence intensity GdAlO_3:Eu becomes stronger. When a part of Gd~(3+) ions is substituted for Y~(3+) ions ,with phase inclining to single GdAlO_3 or YAlO_3, the luminescence intensity becomes stronger according to their emission spectra. They are good substitutes for red powder Y_2O_3:Eu .
At last ,a simple expectation about farther work and direction of this subject was made .
以硝酸铝为主要原料，用碳酸氢铵和氨水作为混合沉淀剂，采用反向滴定共沉淀工艺制备荧光粉体，并对其性能进行研究。研究内容和主要结论如下：
(1)用反向滴定共沉淀工艺制备氧化铝前驱体碳酸铝铵，并对制备工艺进行优化。研究表明：当金属铝盐溶液浓度控制在0.2mol／L，pH值为3～4之间：混合沉淀剂溶液浓度为2mol／L，pH值控制在9～10之间。碳酸氢铵与金属铝盐摩尔比为10，采用反向滴定缓慢(小于0.8L／h)加入的方法，可以得到团聚较少、物相单一、性能优良的前驱体碳酸铝铵。
(2)在不同温度下煅烧前驱体碳酸铝铵，利用TG-DSC，XRD研究其相变过程，得到碳酸铝铵的相变过程为：碳酸铝铵→非晶态氧化铝→γ→氧化铝→θ-氧化铝→α-氧化铝。通过激发光谱和发射光谱分析得到：监测波长为395nm时，氧化铝基体的激发光谱是以247nm为中心220nm到270nm的宽带激发；用254nm波长激发的发射光谱，是以395nm为中心340nm到460nm的宽带发射，发光峰位并不随着煅烧温度的变化而发生变化。而发光强度却有很大的变化，这是内部两种不同作用机制对F~+色心(氧空穴)发光的影响造成的。随着激发波长的增大，发射光谱的主峰位有了一定红移。
(3)制备了Al_2O_3：Eu和Al_2O_3：Eu、Tb发光粉体，利用TG-DSC，XRD，SEM和荧光分光光度计对其相变和发光特性进行研究，得出：稀土Eu、Tb的加入对氧化铝的相变有很大抑制作用，增强了γ-Al_2O_3的热稳定性，掺杂量越多对氧化铝的相变及结晶过程影响越大。Al_2O_3：Eu发光粉体，在掺杂量为1mol％，煅烧温度为1050℃，煅烧时间为4h时，得到发光强度最大的红色荧光粉。通过实验和分析，粉体的主要发射峰(614nm)是Eu~(3+)离子~5D_0-~7F_2能级的跃迁。Tb的掺入，提高了其发光强度，最佳掺杂量为5mol％。
(4)制备和研究了GdAlO_3：Eu和(Gd，Y)AlO_3：Eu发光粉体，利用TG-DSC，XRD和荧光分光光度计对其相变和发光特性进行研究，得出：1200℃煅烧2h即可得到物相单一，发光强度良好的荧光粉体。在Eu掺杂量为3mol％时，GdAlO_3：Eu发光粉体的主要发射峰609nm(~5D_0→~7F_2)强度最大。随着煅烧温度的升高，发射强度增大，到1200℃最大。用Y~(3+)替代部分Gd~(3+)离子时，从发射光谱图表现来看，越是趋向于单一的GdAlO_3或者YAlO_3相时，发光强度越大。它们是很好的红粉Y_2O_3：Eu的替代产品。
最后，对进一步的研究工作和研究方向作了展望。
At the beginning ,according to the basic knowledge about phylogeny , definition , makeup , sorts , luminescent mechanism , preparing methods and applications of luminescence materials ,current research information and subsistent problems of luminescence materials at home and abroad were analyzed in this paper . Red fluorescence powders that use alumina as the matrix were regarded as our research emphases in order to reduce the price of red powders commercially and improve its performances .Research contents and results are as follows:
Fluorescence powders were prepared by using Al(NO_3)-3·9H_2O as the main raw material and using NH_4HCO_3 and urea as the mixed precipitator to adoptthe reverse titration co-precipitation technology . Its performances were studied. The paper consists of four main parts .
Firstly , the precursor NH_4AlO(OH)HCO_3 was prepared by this method that has been optimized. The study about preparing the precursor NH_4AlO(OH)HCO_3(indicates : when the concentration and the pH value of Al(NO_3)_3 solution are 0.2mol/L and 3～4 respectively ;when the concentration and the pH value of the mixed precipitator are 2mol/L and 9～10 respectively ;when the molar ratio of NH_4HCO_3 and Al(NO_3)_3 is 10 , the well dispersive , single phase and excellent performance precursor NH_4AlO(OH)HCO_3 can be obtained by the reverse slow titration (less than 0. 8L/h).
Secondly ,the phase change of powders that were obtained by calcining the precursor NH_4AlO(OH)HCO_3 at different temperatures was studied through TG-DSC and XRD . The process of phase change is that : NH_4AlO(OH)HCO_3→amorphous alumina→γ-alumina→θ-alumina→α-alumina . Through excitation spectra and emission spectra of powders , we get that : When detected at wavelength 395nm ,excitation spectra of alumina matrix is a broad band from 220nm to 270nm at the center of 247nm . Under 254nm excitation, emission spectra of alumina matrix is also a broad band from 340nm to 460nm at the center of 395nm .When the calcining temperatures change ,the location of the peak does not change ,but the intensity changes strongly . The reason is that the luminescence intensity of F~+ color center is effected by the two different mechanisms .When the excitation wavelength becomes bigger , the main peak of emission spectra has some red shift.
Thirdly , the luminescence powders of Al_2O_3: Eu and Al_2O_3:Eu、Tb were prepared . Through TG-DSC, XRD, SEM and fluorescence spectrophotometer, their phases and luminescence property were studied .The results are that :When adding the rare earths of Eu or Tb , the phase change is greatly restrained and the thermal stability ofγ-Al_2O_3 becomes stronger . Adding quantity is more , the effects to the phase change and the crystallization process of alumina are bigger .When the Al_2O_3:Eu powder is calcined at 1050℃for 4h and concentration of Eu~(3+) dopant is 1mol% , Red fluorescence powder Al_2O_3:Eu that has the strongest luminescence intensity is obtained .Through experiments and analysis , the main peak at 614nm is the ~5D_0- ~7F_2 transition of Eu~(3+) ions . Adding Tb can improve the luminescence intensity of Al_2O_3: Eu powder. The optimum concentration of Tb~(3+) dopant is 5mol% .
Fourthly , the luminescence powders of GdAlO_3:Eu and (Gd,Y)AlO_3:Eu were prepared and studied . Through TG-DSC, XRD and fluorescence spectrophotometer, their phases and luminescence property were studied . The results are that : The GdAlO_3:Eu powder calcined at 1200℃for 2h has high luminescence intensity and pure phase . When optimum concentration of Eu~(3+) dopant is 3mol%, the main emission peak is at 609nm (~5D_0→~7F_2) under 254nm excitation .With the calcining temperature increasing ,the luminescence intensity GdAlO_3:Eu becomes stronger. When a part of Gd~(3+) ions is substituted for Y~(3+) ions ,with phase inclining to single GdAlO_3 or YAlO_3, the luminescence intensity becomes stronger according to their emission spectra. They are good substitutes for red powder Y_2O_3:Eu .
At last ,a simple expectation about farther work and direction of this subject was made .
引文
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