稀土掺杂M-Si-Al-O-N材料的合成及其发光特性研究
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摘要
自从以GaN蓝色发光二极管(Light Emitting Diode,简称LED)为基础开发出白光LED照明器件以来,白光LED逐渐发展成一种重要的固态照明光源。白光LED相对于传统白炽灯和荧光灯具有节能、环保、体积小、响应快、寿命长等突出优点。实现白光LED的一种主流方式是紫外或蓝光LED芯片与荧光材料组合,即称为“荧光转换”技术。荧光材料是白光LED必不可少的部分,它直接影响到白光LED的光效、色温、显色指数、光衰和寿命等。传统荧光材料主要是由硫化物、硅酸盐、铝酸盐等构成。近年来,稀土掺杂氮化物和氮氧化物作为一类新型荧光材料,受到人们的密切关注。相对于传统荧光材料来说,在氮化物和氮氧化物基质材料中,氮元素具有相对较小的电负性和较大的电子云膨胀效应,能有效促进稀土离子5d能级在晶体场中的霹裂,使5d-4f之间的能级差减小,导致激发和发射波长红移,能够更好的与紫外或蓝光LED芯片匹配。另外,还具有稳定的化学性质和优良的高温发光性能。但是,目前氮化物和氮氧化物荧光材料存在着制备难度大,以至于对其发光机理研究不够完善的问题。本文主要针对上述问题,在几种氮氧化物荧光材料的合成及其稀土掺杂发光机理研究方面做了一些工作,主要内容有：
(1)结合高温固相和碳热还原法,用低成本的原料,常压下1600℃合成了Ca-a-SiAlON:Eu2+橙黄色荧光材料。最终获得的样品是结晶性很好的单相。由光谱分析可知,它在近紫外和蓝光区域有强吸收,发射谱是500～700nm的宽带,与蓝光LED芯片结合可实现暖白光发射(色温3270～2260K)
(2)通过调整MxV+Si12-(m+n)Alm+nOnN16-n通式中O的含量,制备了Ca1.8Si8.2Al3.7N16:Eu2+荧光材料。单相样品的激发谱与近紫外或蓝光LED芯片相匹配,发射峰在580～601nm之间,对比发现Ca1.8Si8.2Al3.7N16:Eu2+的发光性能要优于Ca-a-SiAlON:Eu2+。
(3)以纳米Si3N4和A1203为原料,常压下,1600℃制备得到了P-SiAlON,在此基础上分别考察Ce3+、Tb3+、Sm2+、Dy3+的发光特性。发现Ce3+和Tb3+共掺时,Ce3+对Tb3+有能量传递；Sm2+的发射谱由锐锋和宽带共同组成,前者属于Sm2+的5Dj→7Fj跃迁,后者是4f55d1→4f6跃迁；Dy3+在P-SiAlON中的发光颜色接近白光。另外,发现Yb/Ho和Yb/Er在P-SiAlON中有上转换现象。
(4)通过高温固相法制备了Ce3+掺杂的Y4S12O7N2荧光材料。在合成单相样品的基础上,详细论述了Y4Si2O7N2的晶体结构。研究发现随着掺杂浓度的改变,样品的发射光可实现从蓝色(-450nm)到绿色(～515nm)的可调,发射光谱的红移主要可以从两方面理解,即晶体场劈裂和再吸收。
Since the first white light-emitting diode (LED) based on the InGaN chip was developed, white LED technique has gradually developed into an important kind of solid-state illumination, In comparison with conventional incandescent and fluorescent lamps, the white LEDs show many projecting advantages such as energy saving, environment friendly, small volume, short response time, long life time and so on. The most commonly method is to combine a phosphor with a GaN LED chip, and this is called as phosphor-conversion method. As an essential part, phoshphors strongly affect the quality of LEDs, such as luminous efficiency, color temperature, color rendering index, life time and so on. So the phosphor is very important in white light LED. Traditional phosphors usually based on the sulfide, aluminate and silicate. In recent years, the rare-earth doped (oxy)nitride phosphors have attracted much attention. In (oxy)nitride phosphors, the nephelauxetic effect and the relative low electronegativity value of N3-ion cause the large splitting of5d energy levels, which makes the redshift of the excitation and emission band, so it makes them as a potential candidate for the UV-LED and blue LED. The (oxy)nitride phosphors also have the advantages of better flexibility, composition-tunability and higher thermal and chemical stability. But the preparation of (oxy)nitride phosphors is very difficult and the luminescence mechanism have not been studied deeply.So this thesis focuses on the preparation of several oxynitride phosphors and the luminescence mechanism. The main works were contained as below:
(l)Yellow-orange oxynitride Ca-a-SiAlON:Eu2+phosphors with the compositions of Cao.8Si9.2Al2.8O1.2N14.8:xEu2+(x=0-0.24) were obtained via carbothermal reduction and nitridation method. The XRD analysis indicated the high purity and crystalline of sample, and no residual carbon existed. The resulting phosphors can absorb light in the range of300～500nm efficiently and show a single intense broad emission band in the wavelength range of500-700nm. It reveals that Ca-a-SiAlON:Eu2+is a good candidate for warm white-LEDs (color temperatures,3270-2260K).
(2)Cai.8Si8.2Al3.7N16:Eu2+phosphor was abtained by changing the oxygen content of general formula Mxv+Si12-(m+n)Alm+OnnN16-n. The samples could efficiently excited by near ultraviolet or blue LED chip, and show a single intense broad emission band at580～601nm. By contrast, the luminescence properties of Ca1.8Si8.2Al3.7Ni6:Eu2+are better than Ca-a-SiA1ON:Eu2+.
(3)Rare-earth-doped P-SiAlON phosphors, with the compositions of Si6-zAlzOzN8-z:Re (z=1, Re=Ce3+, Tb3+, Sm2+and Dy3+), were prepared by a solid-state reaction at1600℃under atmospheric pressure. The energy transfer from Ce3+to Tb3+ions in Si5A1ON7:Ce3+,Tb3+has been studied. The emission spectra consist of broad band and line peaks at room temperature, which are ascribed to the4f55d1→4f6and5Do→7FJ transitions of Sm2+respectively. Dy3+doped β-SiA1ON emits approximate white light. In addition, the up-conversion luminescence properties have been studied firstly in β-SiAlON:Ln3+(Ln=Yb/Ho, Yb/Er)
(4)Y4Si2O7N2:Ce3+was synthesized using a solid-state reaction and its crystal structure was introduced in detail. Ce3+-doped Y4Si2O7N2exhibited a broad emission band and the maximum emission wavelength could be tuned from blue (λem=450nm) to green (λem=515nm) by increasing the concentration of Ce3+. The red-shifting behavior is mainly attributed to two factors:crystal field strengthening and radiation re-absorption of the high energy emission.
(1)结合高温固相和碳热还原法,用低成本的原料,常压下1600℃合成了Ca-a-SiAlON:Eu2+橙黄色荧光材料。最终获得的样品是结晶性很好的单相。由光谱分析可知,它在近紫外和蓝光区域有强吸收,发射谱是500～700nm的宽带,与蓝光LED芯片结合可实现暖白光发射(色温3270～2260K)
(2)通过调整MxV+Si12-(m+n)Alm+nOnN16-n通式中O的含量,制备了Ca1.8Si8.2Al3.7N16:Eu2+荧光材料。单相样品的激发谱与近紫外或蓝光LED芯片相匹配,发射峰在580～601nm之间,对比发现Ca1.8Si8.2Al3.7N16:Eu2+的发光性能要优于Ca-a-SiAlON:Eu2+。
(3)以纳米Si3N4和A1203为原料,常压下,1600℃制备得到了P-SiAlON,在此基础上分别考察Ce3+、Tb3+、Sm2+、Dy3+的发光特性。发现Ce3+和Tb3+共掺时,Ce3+对Tb3+有能量传递；Sm2+的发射谱由锐锋和宽带共同组成,前者属于Sm2+的5Dj→7Fj跃迁,后者是4f55d1→4f6跃迁；Dy3+在P-SiAlON中的发光颜色接近白光。另外,发现Yb/Ho和Yb/Er在P-SiAlON中有上转换现象。
(4)通过高温固相法制备了Ce3+掺杂的Y4S12O7N2荧光材料。在合成单相样品的基础上,详细论述了Y4Si2O7N2的晶体结构。研究发现随着掺杂浓度的改变,样品的发射光可实现从蓝色(-450nm)到绿色(～515nm)的可调,发射光谱的红移主要可以从两方面理解,即晶体场劈裂和再吸收。
Since the first white light-emitting diode (LED) based on the InGaN chip was developed, white LED technique has gradually developed into an important kind of solid-state illumination, In comparison with conventional incandescent and fluorescent lamps, the white LEDs show many projecting advantages such as energy saving, environment friendly, small volume, short response time, long life time and so on. The most commonly method is to combine a phosphor with a GaN LED chip, and this is called as phosphor-conversion method. As an essential part, phoshphors strongly affect the quality of LEDs, such as luminous efficiency, color temperature, color rendering index, life time and so on. So the phosphor is very important in white light LED. Traditional phosphors usually based on the sulfide, aluminate and silicate. In recent years, the rare-earth doped (oxy)nitride phosphors have attracted much attention. In (oxy)nitride phosphors, the nephelauxetic effect and the relative low electronegativity value of N3-ion cause the large splitting of5d energy levels, which makes the redshift of the excitation and emission band, so it makes them as a potential candidate for the UV-LED and blue LED. The (oxy)nitride phosphors also have the advantages of better flexibility, composition-tunability and higher thermal and chemical stability. But the preparation of (oxy)nitride phosphors is very difficult and the luminescence mechanism have not been studied deeply.So this thesis focuses on the preparation of several oxynitride phosphors and the luminescence mechanism. The main works were contained as below:
(l)Yellow-orange oxynitride Ca-a-SiAlON:Eu2+phosphors with the compositions of Cao.8Si9.2Al2.8O1.2N14.8:xEu2+(x=0-0.24) were obtained via carbothermal reduction and nitridation method. The XRD analysis indicated the high purity and crystalline of sample, and no residual carbon existed. The resulting phosphors can absorb light in the range of300～500nm efficiently and show a single intense broad emission band in the wavelength range of500-700nm. It reveals that Ca-a-SiAlON:Eu2+is a good candidate for warm white-LEDs (color temperatures,3270-2260K).
(2)Cai.8Si8.2Al3.7N16:Eu2+phosphor was abtained by changing the oxygen content of general formula Mxv+Si12-(m+n)Alm+OnnN16-n. The samples could efficiently excited by near ultraviolet or blue LED chip, and show a single intense broad emission band at580～601nm. By contrast, the luminescence properties of Ca1.8Si8.2Al3.7Ni6:Eu2+are better than Ca-a-SiA1ON:Eu2+.
(3)Rare-earth-doped P-SiAlON phosphors, with the compositions of Si6-zAlzOzN8-z:Re (z=1, Re=Ce3+, Tb3+, Sm2+and Dy3+), were prepared by a solid-state reaction at1600℃under atmospheric pressure. The energy transfer from Ce3+to Tb3+ions in Si5A1ON7:Ce3+,Tb3+has been studied. The emission spectra consist of broad band and line peaks at room temperature, which are ascribed to the4f55d1→4f6and5Do→7FJ transitions of Sm2+respectively. Dy3+doped β-SiA1ON emits approximate white light. In addition, the up-conversion luminescence properties have been studied firstly in β-SiAlON:Ln3+(Ln=Yb/Ho, Yb/Er)
(4)Y4Si2O7N2:Ce3+was synthesized using a solid-state reaction and its crystal structure was introduced in detail. Ce3+-doped Y4Si2O7N2exhibited a broad emission band and the maximum emission wavelength could be tuned from blue (λem=450nm) to green (λem=515nm) by increasing the concentration of Ce3+. The red-shifting behavior is mainly attributed to two factors:crystal field strengthening and radiation re-absorption of the high energy emission.
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