Y_2O_3：Eu~（3+）纳米粉末和透明陶瓷的制备及光谱性质研究
摘要
本论文包含四章内容,绪论介绍了论文工作的背景;第2章到第4章报道了Y_2O_3∶Eu~(3+)纳米粉末和透明陶瓷的制备、形貌结构表征及发光性质研究结果.
绪论首先介绍了近几年重点研究的一些稀土发光材料,然后详细阐述了光致发光的基本原理和三价稀土离子的发光特性,并给出透明陶瓷的相关知识:最后简单讨论了利用溶液燃烧法和均相沉淀法制备纳米粉末的相关内容.
在第2章中,用燃烧法制备Y_2O_3∶Eu~(3+)纳米粉末,研究了前驱溶液pH值的改变对粉末形貌和发光性质的影响。利用XRD和SEM对粉末的结构形貌进行表征,结果显示随着溶液pH值的增大,晶粒逐渐增大,并且晶粒间的团聚变得更厉害,粉末变得更致密,气孔率降低。TG-DZA曲线显示,在高pH值下燃烧持续时间变长可能是导致粉末团聚更厉害的原因。粉末的发射谱由三价Eu~(3+)离子在立方Y_2O_3中的典型发射峰组成,最强的发射位于612 nm,是由~5D_0-~7F_2电偶极跃迁引起的。发射谱显示,随着pH值的增大,样品的发光逐渐增强。激发谱由基质吸收、电荷迁移带和4f组态内的跃迁三部分组成,随着pH值的增大,基质吸收相对电荷迁移带的激发强度逐渐减弱。样品的荧光寿命测量结果表明,pH值越大,即晶粒越大,荧光寿命越短。
由于燃烧法制备的粉末中存在不利于透明陶瓷烧结的团聚现象,在本章的第二部分研究了PEG2000分散剂的使用对粉末形貌和光谱性质的影响。少量分散剂的加入,使得粉末的晶粒有些微增大,但是随着用量的继续增加,晶粒逐渐减小。最重要的是,适量(10wt%)分散剂可以使粉末中的团聚体尺寸明显减小。同时,发射光谱表明,在晶粒大小相同甚至更小的情况下,团聚体的减小使样品的发光明显增强。激发谱中出现随着晶粒减小,电荷迁移带红移的现象,这是由于表面态上的Eu-O键变长,共价性减弱的结果。荧光寿命测量的结果显示,晶粒大小相差一倍的粉末几乎具有相同的寿命。
第3章中采用改善的凝胶燃烧法制备Y_2O_3∶Eu~(3+)粉末,与直接燃烧得到的粉末进行对比,并利用这些粉末采用真空和氮气烧结相结合的方法制备透明陶瓷,观察粉末性质的不同对透明陶瓷微观结构的影响。粉末的XRD分析表明,凝胶过程对晶粒的大小几乎没有影响,与直接燃烧一样,晶粒大小主要由甘氨酸和金属离子的摩尔比决定。但是,SEM和TEM图显示,燃烧前的凝胶过程可以显著地减小团聚体的尺寸。陶瓷的表面形貌图表明,粉末中的团聚体越小,陶瓷的微观结构越均匀,表面越平整。而以直接燃烧制备的样品为前驱粉末烧结的陶瓷不仅表面凹凸不平,而且出现了裂纹和气孔,对陶瓷的透明度产生致命影响。光谱分析显示,陶瓷和粉末的发射谱除强度不同外,谱型完全相同,而两者的激发谱则存在一些差异。
第4章中采用均相沉淀法制备Y_2O_3∶Eu~(3+)粉末,并将其烧结为透明陶瓷。结构和形貌分析显示,在本论文的实验条件范围内,反应物浓度、水浴温度和煅烧温度对样品形貌和结构的影响很小,得到的粉末都是由小晶粒团聚成的大于100nm的球形颗粒组成。但是,溶液pH值的不同可以显著改变粉末的形貌。调节溶液的pH值为6.5,则制备得到的粉末晶粒不会团聚成大颗粒,分散性较好,由此烧结而成的陶瓷也具有更好的透明度。陶瓷的表面SEM图显示,由于粉末中存在团聚体,烧结得到的陶瓷晶粒大小和形貌很不均匀,而分散性较好的粉末则可以得到微观结构均匀的陶瓷样品。陶瓷和粉末的荧光衰减曲线显示,前者的荧光寿命比后者短的多.
This thesis focuses on the preparation and spectral properties of Y_2O_3:Eu~(3+) nano-powders and ceramics,which is composed of four chapters.In the preface,the background of my work is introduced.In chapter 2 to 4,the synthesis of Y_2O_3:Eu~(3+) nano-powders and ceramics as well as the morphological,structural and spectral properties of the resultant samples are repoted.
In chapter 1,an introduction of some important rare earth luminescent materials is given at first.Then the basic principals ofphotoluminescence,spectral properties of trivalent rare-earth ions as well as knowledge of transparent ceramics are stated.At last,combustion and homogeneous precipitation methods for synthesis of nano-powders are briefly introduced.
In chapter 2,Y_2O_3:Eu~(3+) nano-powders were synthesized by combustion method and the influence of pH value on properties of combustion-derived powders was studied.The structure and morphology analyses display that with the increase of pH value,the crystallites become bigger,and the powder becomes more and more compact.TG-DAT curves indicate that longer combustion time is needed under higher pH value,which may account for the severer agglomeration in corresponding powders. The emission spectra of powders contain the typical Eu~(3+) luminescent components in cubic Y_2O_3 with the strongest emission at 612 nm assigned to ~5D_0-~7F_2 forced electric dipole transition.The emission spectra show that with the increase of pH value,the luminescent intensity of Y_2O_3:Eu~(3+) nano-powder is enhanced.The excitation spectra consist of three parts:host absorption,charge transfer band and transition within 4f orbital and the relative intensity of host absorption weakens with the increase of pH value.The decay curves reveal the observed lifetime of Y_2O_3:Eu~(3+) nano-powder shortens with the increase of crystalline size.
Agglomeration,which is deleterious to the transparency of ceramic,is easily present in the powders prepared by combustion method,so PEG2000 was used as dispersant to improve the dispersivity of the resultant powders.Small amount of dispersant increases the crystalline size slightly,while with the continuous increase of dispersant,the crystallites become smaller and smaller.What is the most important is that appropriate amount of dispersant(10wt%) reduces the size of agglomerate obviously.Emission spectra confirm that the reduction of agglomerate size can enhance the luminescent intensity apparently when the powders possess almost the same crystalline size.In the excitation spectra,red-shift of charge transfer band with the decrease of crystalline size is observed,resulting from the increase of surface area. The decay curves reveal that powders with different crystalline size have almost the same lifetime.
In chapter 3,Y_2O_3:Eu~(3+)nano-powders were prepared by gel combustion,and the products were compared with those produced by direct combustion.The resultant powders were sintered into transparent ceramics and the influence of properties of powders on microstructures of ceramics was studied.XRD analysis indicates the gel process before combustion has no influence on the crystalline size,which is mainly determined by the molar ratio of glycine to metal ions.However,TEM and SEM images reveal that the gel process can reduce the size of agglomerate significantly. The surface morphologies of ceramics show that smaller agglomerates lead to even surface and homogeneous structure while cracks and pores are present in the ceramics derived from powders prepared by direct combustion.Powders and the corresponding ceramics have just the same emission spectra in terms of peak position.But there are some distinct differences in the excitation spectra.
In chapter 4,homogeneous precipitation was used to prepare Y_2O_3:Eu~(3+) nano-powders,which were subsequently sintered into ceramics.In the experiment condition range of this thesis,it is found that the concentration of reactant,the water-bath temperature and calcination temperature have no significant influence on the morphologies and structures of the resultant powders,all of which are composed of crystallite-agglomerated spherical particles.Nevertheless,the pH value of solution makes striking difference.When the pH value of solution was adjusted to 6.5,the synthesized powder has good dispersivity and the corresponding ceramic shows better transparency.SEM images of ceramics confirm that agglomeration in powder results in wide crystalline size distribution and heterogeneous morphology while good dispersivity ensures homogeneous microstructure.The decay curves of ceramic and powder reveal that former has much shorter lifetime.
绪论首先介绍了近几年重点研究的一些稀土发光材料,然后详细阐述了光致发光的基本原理和三价稀土离子的发光特性,并给出透明陶瓷的相关知识:最后简单讨论了利用溶液燃烧法和均相沉淀法制备纳米粉末的相关内容.
在第2章中,用燃烧法制备Y_2O_3∶Eu~(3+)纳米粉末,研究了前驱溶液pH值的改变对粉末形貌和发光性质的影响。利用XRD和SEM对粉末的结构形貌进行表征,结果显示随着溶液pH值的增大,晶粒逐渐增大,并且晶粒间的团聚变得更厉害,粉末变得更致密,气孔率降低。TG-DZA曲线显示,在高pH值下燃烧持续时间变长可能是导致粉末团聚更厉害的原因。粉末的发射谱由三价Eu~(3+)离子在立方Y_2O_3中的典型发射峰组成,最强的发射位于612 nm,是由~5D_0-~7F_2电偶极跃迁引起的。发射谱显示,随着pH值的增大,样品的发光逐渐增强。激发谱由基质吸收、电荷迁移带和4f组态内的跃迁三部分组成,随着pH值的增大,基质吸收相对电荷迁移带的激发强度逐渐减弱。样品的荧光寿命测量结果表明,pH值越大,即晶粒越大,荧光寿命越短。
由于燃烧法制备的粉末中存在不利于透明陶瓷烧结的团聚现象,在本章的第二部分研究了PEG2000分散剂的使用对粉末形貌和光谱性质的影响。少量分散剂的加入,使得粉末的晶粒有些微增大,但是随着用量的继续增加,晶粒逐渐减小。最重要的是,适量(10wt%)分散剂可以使粉末中的团聚体尺寸明显减小。同时,发射光谱表明,在晶粒大小相同甚至更小的情况下,团聚体的减小使样品的发光明显增强。激发谱中出现随着晶粒减小,电荷迁移带红移的现象,这是由于表面态上的Eu-O键变长,共价性减弱的结果。荧光寿命测量的结果显示,晶粒大小相差一倍的粉末几乎具有相同的寿命。
第3章中采用改善的凝胶燃烧法制备Y_2O_3∶Eu~(3+)粉末,与直接燃烧得到的粉末进行对比,并利用这些粉末采用真空和氮气烧结相结合的方法制备透明陶瓷,观察粉末性质的不同对透明陶瓷微观结构的影响。粉末的XRD分析表明,凝胶过程对晶粒的大小几乎没有影响,与直接燃烧一样,晶粒大小主要由甘氨酸和金属离子的摩尔比决定。但是,SEM和TEM图显示,燃烧前的凝胶过程可以显著地减小团聚体的尺寸。陶瓷的表面形貌图表明,粉末中的团聚体越小,陶瓷的微观结构越均匀,表面越平整。而以直接燃烧制备的样品为前驱粉末烧结的陶瓷不仅表面凹凸不平,而且出现了裂纹和气孔,对陶瓷的透明度产生致命影响。光谱分析显示,陶瓷和粉末的发射谱除强度不同外,谱型完全相同,而两者的激发谱则存在一些差异。
第4章中采用均相沉淀法制备Y_2O_3∶Eu~(3+)粉末,并将其烧结为透明陶瓷。结构和形貌分析显示,在本论文的实验条件范围内,反应物浓度、水浴温度和煅烧温度对样品形貌和结构的影响很小,得到的粉末都是由小晶粒团聚成的大于100nm的球形颗粒组成。但是,溶液pH值的不同可以显著改变粉末的形貌。调节溶液的pH值为6.5,则制备得到的粉末晶粒不会团聚成大颗粒,分散性较好,由此烧结而成的陶瓷也具有更好的透明度。陶瓷的表面SEM图显示,由于粉末中存在团聚体,烧结得到的陶瓷晶粒大小和形貌很不均匀,而分散性较好的粉末则可以得到微观结构均匀的陶瓷样品。陶瓷和粉末的荧光衰减曲线显示,前者的荧光寿命比后者短的多.
This thesis focuses on the preparation and spectral properties of Y_2O_3:Eu~(3+) nano-powders and ceramics,which is composed of four chapters.In the preface,the background of my work is introduced.In chapter 2 to 4,the synthesis of Y_2O_3:Eu~(3+) nano-powders and ceramics as well as the morphological,structural and spectral properties of the resultant samples are repoted.
In chapter 1,an introduction of some important rare earth luminescent materials is given at first.Then the basic principals ofphotoluminescence,spectral properties of trivalent rare-earth ions as well as knowledge of transparent ceramics are stated.At last,combustion and homogeneous precipitation methods for synthesis of nano-powders are briefly introduced.
In chapter 2,Y_2O_3:Eu~(3+) nano-powders were synthesized by combustion method and the influence of pH value on properties of combustion-derived powders was studied.The structure and morphology analyses display that with the increase of pH value,the crystallites become bigger,and the powder becomes more and more compact.TG-DAT curves indicate that longer combustion time is needed under higher pH value,which may account for the severer agglomeration in corresponding powders. The emission spectra of powders contain the typical Eu~(3+) luminescent components in cubic Y_2O_3 with the strongest emission at 612 nm assigned to ~5D_0-~7F_2 forced electric dipole transition.The emission spectra show that with the increase of pH value,the luminescent intensity of Y_2O_3:Eu~(3+) nano-powder is enhanced.The excitation spectra consist of three parts:host absorption,charge transfer band and transition within 4f orbital and the relative intensity of host absorption weakens with the increase of pH value.The decay curves reveal the observed lifetime of Y_2O_3:Eu~(3+) nano-powder shortens with the increase of crystalline size.
Agglomeration,which is deleterious to the transparency of ceramic,is easily present in the powders prepared by combustion method,so PEG2000 was used as dispersant to improve the dispersivity of the resultant powders.Small amount of dispersant increases the crystalline size slightly,while with the continuous increase of dispersant,the crystallites become smaller and smaller.What is the most important is that appropriate amount of dispersant(10wt%) reduces the size of agglomerate obviously.Emission spectra confirm that the reduction of agglomerate size can enhance the luminescent intensity apparently when the powders possess almost the same crystalline size.In the excitation spectra,red-shift of charge transfer band with the decrease of crystalline size is observed,resulting from the increase of surface area. The decay curves reveal that powders with different crystalline size have almost the same lifetime.
In chapter 3,Y_2O_3:Eu~(3+)nano-powders were prepared by gel combustion,and the products were compared with those produced by direct combustion.The resultant powders were sintered into transparent ceramics and the influence of properties of powders on microstructures of ceramics was studied.XRD analysis indicates the gel process before combustion has no influence on the crystalline size,which is mainly determined by the molar ratio of glycine to metal ions.However,TEM and SEM images reveal that the gel process can reduce the size of agglomerate significantly. The surface morphologies of ceramics show that smaller agglomerates lead to even surface and homogeneous structure while cracks and pores are present in the ceramics derived from powders prepared by direct combustion.Powders and the corresponding ceramics have just the same emission spectra in terms of peak position.But there are some distinct differences in the excitation spectra.
In chapter 4,homogeneous precipitation was used to prepare Y_2O_3:Eu~(3+) nano-powders,which were subsequently sintered into ceramics.In the experiment condition range of this thesis,it is found that the concentration of reactant,the water-bath temperature and calcination temperature have no significant influence on the morphologies and structures of the resultant powders,all of which are composed of crystallite-agglomerated spherical particles.Nevertheless,the pH value of solution makes striking difference.When the pH value of solution was adjusted to 6.5,the synthesized powder has good dispersivity and the corresponding ceramic shows better transparency.SEM images of ceramics confirm that agglomeration in powder results in wide crystalline size distribution and heterogeneous morphology while good dispersivity ensures homogeneous microstructure.The decay curves of ceramic and powder reveal that former has much shorter lifetime.
引文
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