稀土掺杂Ca_2BO_3Cl荧光粉的合成、发光特性及其在白光LEDs中的潜在应用
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摘要
白光LEDs是照明领域的革新者,白光LEDs用荧光粉亦成为发光领域的研究热点之一。本文采用高温固相法,以Ca2BO3Cl为基质,以Eu2+、Ce3+、Tb3+、Eu3+及Sm3+等为激活剂,制备了在白光LEDs领域有潜在应用价值的荧光粉,研究了材料的发光性质。主要研究内容及结果如下：
1、获得了蓝光激发型Ca2BO3Cl:Eu2+黄色发光粉,研究了材料的发光性质。研究发现,在460nm蓝色光激发下,材料呈一非对称的单峰发射,主峰位于573nm,对应Eu2+的4f65d1→4f7跃迁。分析认为,Ca2BO3Cl:Eu2+呈现非对称发射的原因是Eu2+取代Ca2BO3Cl中两种Ca2+格位,形成了两种不同的发光中心。Eu2+的掺杂量影响了材料的发光强度,出现了浓度猝灭现象,猝灭机理为电偶极-电偶极相互作用。利用理论公式计算得到了R。为2.166nm,利用光谱数据,计算得到的Rc为2.120nm,二者符合较好。研究了CaCl2和H3BO3用量对材料发光特性等的影响。结果显示,添加过量的CaCl2或H3BO3,均能提高材料的发射强度,CaCl2和H3BO3最佳的摩尔用量分别为过量5%和15%。将Ca2BO3Cl:Eu2+材料与460nm InGaN芯片组合,获得了白光LEDs,色坐标为(0.339,0.351)。
2、获得了适于紫外-近紫外光激发的发光颜色由蓝-绿可变的Ca2BO3Cl:Ce3+,Tb3+荧光粉。Ce3+、Tb3+在Ca2BO3Cl中分别发射蓝和绿色光,且发射强度随Ce3+和Tb3+掺杂浓度的增大,均表现出先增大、后减小的变化趋势,当Ce3+、Tb3+摩尔掺杂量分别为3%和5%时,强度最大。通过调节Ce3+、Tb3+配比,获得了发光颜色由蓝到绿逐渐变化的Ca2BO3Cl:Ce3+,Tb3+荧光粉,通过Ce3+、Tb3+间的能量传递,可有效提高Tb3+在Ca2BO3Cl材料中的发射强度。结果显示,Ca2BO3Cl:Ce3+,Tb3+是一种在紫外基白光LEDs领域有潜在应用价值的颜色可调型荧光粉。
3、获得了长波紫外光激发型Ca2BO3Cl:Sm3+、Ca2BO3Cl:Eu3+和Ca2BO3Cl:Sm3+,Eu3+荧光粉,研究了材料的发光性质。结果表明,以401nm近紫外光作为激发源时,Ca2BO3Cl:Sm3+材料发射橙红光,主峰位于603nm；以392nm近紫外光作为激发源时,Ca2BO3Cl:Eu3+材料发射红色光,主峰位于623nm,但是,材料在395-405nm波段吸收较弱。添加Sm3+于Ca2BO3Cl:Eu3+材料,发现Sm3+对Eu3+有很好的敏化作用,通过Sm3+对Eu3+的能量传递,有效地改善了Ca2BO3Cl:Sm3+,Eu3+材料在395-405nm区域的吸收特性：通过调整Sm3+掺杂量,明显增强了材料的发射强度,强于商业Y2O2S:0.05Eu3+的发射强度,材料的色坐标接近标准的红色区域。此外,通过记录Sm3+的发射强度随Eu3+掺杂量的变化情况,计算得到Sm3+、Eu3+间能量传递的有效临界距离为2.17nrn。上述研究结果表明Ca2BO3Cl:Sm3+,Eu3+是一种有应用前景的三基色白光LEDs用红色发光粉。
4、获得了Ca2BO3Cl:Tb3+及Ca2BO3Cl:Tb3+,A+(A=Li、Na、K荧光粉,研究了材料的发光特性等。结果显示,添加补偿电荷A+(A=Li、Na,K),可有效地提高Ca2BO3Cl:Tb3+材料的绿色发射强度,补偿电荷为Li+、Na+、K+时,分别提高了1.61、1.97和1.81倍,对应的色坐标为(0.335,0.584)、(0.335,0.585)和(0.335,0.585)。可见,A+(A=Li、Na、K)是能够改善Ca2BO3Cl:Tb3+材料性能的优质补偿电荷,且以Na+为最优。
White LEDs are regarded as the new revolution in the domain of illumination. It is one of the focus that the phosphors which are used for white LEDs in the region of the luminescent materials. In this research, Eu2+, Ce3+, Tb3+, Eu3+or Sm3+doped Ca2BO3Cl phosphors are synthesized by a high temperature solid-state method, and its luminescent properties are investigated. The results show that the phosphors may have a potential application in white LEDs. The research and results are summarized as follows:
Ca2BO3Cl:Eu2+produce a yellow emission under the ultraviolet and blue radiation excitation. Because Eu2+may occupy two types of Ca2+sites, Ca2BO3Cl:Eu2+emits an asymmetrical single intensive band at573nm corresponding to the4f65d1→4f7transition of Eu2+. With an increase the Eu2+doping content, the emission intensity of Ca2BO3Cl:Eu2+is influenced, the concentration quenching is obviously observed, and its mechanism is verified to be a dipole-dipole interaction. The value of the critical transfer distance is calculated as2.166nm, which is in good agreement with the value2.120nm derived from the experimental data. The luminescent properties of Eu2+doped Ca2BO3Cl are influenced by CaCl2and H3BO3. Its emission intensity can be enhanced by adding the excess of CaCl2and H3BO3, and the optimal excess mole concentrations are5mol%and15mol%, respectively. White LEDs are fabricated with Ca2BO3Cl:Eu2+and460nm LED chip, and the CIE chromaticity coordinates is (0.339,0.351).
Ca2BO3Cl:Ce3+, Tb3+can produce emission color from blue to green under the ultraviolet radiation excitation. Ce3+and Tb3+in Ca2BO3Cl can produce blue and green light, respectively. And their emission intensities firstly increase, then decrease with the increasing Ce3+and Tb3+doping content, and reach the maximum value at3%Ce3+and5%Tb3+, respectively. Ca2BO3Cl:Ce3+, Tb3+can emit color from blue to green by tuning the relative ratio of Ce3+and Tb3+, and the emission intensity of Tb3+in Ca2BO33Cl can be enhanced by the energy transfer from Ce3+to Tb3+. The results show Ca2BO3Cl:Ce3+, Tb3+may be promising tuning emission phosphor for white LEDs.
Sm3+, Eu3+or Sm3+/Eu3+doped Ca2BO3Cl phosphor can be excited by the long ultraviolet radiation excitation. Ca2BO3Cl:Sm3+can produce orange-red light (603nm) under401nm radiation excitation. Ca2BO3Cl:Eu3+can show red light (623nm) under392nm radiation excitation, however, it has a low absorption in the region of395-405nm. The emission intensity of Eu3+in Ca2BO3Cl can be enhanced by codoping Sm3+as a sensitizer, and the energy transfer efficiency (Sm3+→Eu3+) gradually increases to55%by increasing Eu3+doping content. It is found to be efficient to extend and strengthen the absorption of near-ultraviolet light in the region of395-405nm by codoping Sm3+. Moreover, the chromaticity coordinates of Ca2BO3Cl:Sm3+, Eu3+can also be influenced by the molar concentration of Eu3+, and the emission intensity and CIE can be compared to those of the conventional red phosphor Y2O2S:Eu3+. The result show Ca2BO3Cl:Sm3+, Eu3+may be promising red emitting phosphor for white LEDs.
Ca2BO3Cl:Tb3+and Ca2BO3Cl:Tb3+, A+(A=Li, Na, K) phopshors are prepared, and their luminescent properties are investigated.The emission intensity of Ca2BO3Cl:Tb3+can be enhanced about1.61,1.97and1.81times by codoping compersation charge Li+, Na+and K+, respectively, and the CIE chromaticity coordinates of Ca2BO3Cl:Tb3+, A+(A=Li,Na, K) are (0.335,0.584),(0.335,0.585) and (0.335,0.585), respectively. Hence, A+(A=Li, Na, K) may be the optimal charge compensator for Ca2BO3Cl:Tb3+, and Na+has the optimal effect.
1、获得了蓝光激发型Ca2BO3Cl:Eu2+黄色发光粉,研究了材料的发光性质。研究发现,在460nm蓝色光激发下,材料呈一非对称的单峰发射,主峰位于573nm,对应Eu2+的4f65d1→4f7跃迁。分析认为,Ca2BO3Cl:Eu2+呈现非对称发射的原因是Eu2+取代Ca2BO3Cl中两种Ca2+格位,形成了两种不同的发光中心。Eu2+的掺杂量影响了材料的发光强度,出现了浓度猝灭现象,猝灭机理为电偶极-电偶极相互作用。利用理论公式计算得到了R。为2.166nm,利用光谱数据,计算得到的Rc为2.120nm,二者符合较好。研究了CaCl2和H3BO3用量对材料发光特性等的影响。结果显示,添加过量的CaCl2或H3BO3,均能提高材料的发射强度,CaCl2和H3BO3最佳的摩尔用量分别为过量5%和15%。将Ca2BO3Cl:Eu2+材料与460nm InGaN芯片组合,获得了白光LEDs,色坐标为(0.339,0.351)。
2、获得了适于紫外-近紫外光激发的发光颜色由蓝-绿可变的Ca2BO3Cl:Ce3+,Tb3+荧光粉。Ce3+、Tb3+在Ca2BO3Cl中分别发射蓝和绿色光,且发射强度随Ce3+和Tb3+掺杂浓度的增大,均表现出先增大、后减小的变化趋势,当Ce3+、Tb3+摩尔掺杂量分别为3%和5%时,强度最大。通过调节Ce3+、Tb3+配比,获得了发光颜色由蓝到绿逐渐变化的Ca2BO3Cl:Ce3+,Tb3+荧光粉,通过Ce3+、Tb3+间的能量传递,可有效提高Tb3+在Ca2BO3Cl材料中的发射强度。结果显示,Ca2BO3Cl:Ce3+,Tb3+是一种在紫外基白光LEDs领域有潜在应用价值的颜色可调型荧光粉。
3、获得了长波紫外光激发型Ca2BO3Cl:Sm3+、Ca2BO3Cl:Eu3+和Ca2BO3Cl:Sm3+,Eu3+荧光粉,研究了材料的发光性质。结果表明,以401nm近紫外光作为激发源时,Ca2BO3Cl:Sm3+材料发射橙红光,主峰位于603nm；以392nm近紫外光作为激发源时,Ca2BO3Cl:Eu3+材料发射红色光,主峰位于623nm,但是,材料在395-405nm波段吸收较弱。添加Sm3+于Ca2BO3Cl:Eu3+材料,发现Sm3+对Eu3+有很好的敏化作用,通过Sm3+对Eu3+的能量传递,有效地改善了Ca2BO3Cl:Sm3+,Eu3+材料在395-405nm区域的吸收特性：通过调整Sm3+掺杂量,明显增强了材料的发射强度,强于商业Y2O2S:0.05Eu3+的发射强度,材料的色坐标接近标准的红色区域。此外,通过记录Sm3+的发射强度随Eu3+掺杂量的变化情况,计算得到Sm3+、Eu3+间能量传递的有效临界距离为2.17nrn。上述研究结果表明Ca2BO3Cl:Sm3+,Eu3+是一种有应用前景的三基色白光LEDs用红色发光粉。
4、获得了Ca2BO3Cl:Tb3+及Ca2BO3Cl:Tb3+,A+(A=Li、Na、K荧光粉,研究了材料的发光特性等。结果显示,添加补偿电荷A+(A=Li、Na,K),可有效地提高Ca2BO3Cl:Tb3+材料的绿色发射强度,补偿电荷为Li+、Na+、K+时,分别提高了1.61、1.97和1.81倍,对应的色坐标为(0.335,0.584)、(0.335,0.585)和(0.335,0.585)。可见,A+(A=Li、Na、K)是能够改善Ca2BO3Cl:Tb3+材料性能的优质补偿电荷,且以Na+为最优。
White LEDs are regarded as the new revolution in the domain of illumination. It is one of the focus that the phosphors which are used for white LEDs in the region of the luminescent materials. In this research, Eu2+, Ce3+, Tb3+, Eu3+or Sm3+doped Ca2BO3Cl phosphors are synthesized by a high temperature solid-state method, and its luminescent properties are investigated. The results show that the phosphors may have a potential application in white LEDs. The research and results are summarized as follows:
Ca2BO3Cl:Eu2+produce a yellow emission under the ultraviolet and blue radiation excitation. Because Eu2+may occupy two types of Ca2+sites, Ca2BO3Cl:Eu2+emits an asymmetrical single intensive band at573nm corresponding to the4f65d1→4f7transition of Eu2+. With an increase the Eu2+doping content, the emission intensity of Ca2BO3Cl:Eu2+is influenced, the concentration quenching is obviously observed, and its mechanism is verified to be a dipole-dipole interaction. The value of the critical transfer distance is calculated as2.166nm, which is in good agreement with the value2.120nm derived from the experimental data. The luminescent properties of Eu2+doped Ca2BO3Cl are influenced by CaCl2and H3BO3. Its emission intensity can be enhanced by adding the excess of CaCl2and H3BO3, and the optimal excess mole concentrations are5mol%and15mol%, respectively. White LEDs are fabricated with Ca2BO3Cl:Eu2+and460nm LED chip, and the CIE chromaticity coordinates is (0.339,0.351).
Ca2BO3Cl:Ce3+, Tb3+can produce emission color from blue to green under the ultraviolet radiation excitation. Ce3+and Tb3+in Ca2BO3Cl can produce blue and green light, respectively. And their emission intensities firstly increase, then decrease with the increasing Ce3+and Tb3+doping content, and reach the maximum value at3%Ce3+and5%Tb3+, respectively. Ca2BO3Cl:Ce3+, Tb3+can emit color from blue to green by tuning the relative ratio of Ce3+and Tb3+, and the emission intensity of Tb3+in Ca2BO33Cl can be enhanced by the energy transfer from Ce3+to Tb3+. The results show Ca2BO3Cl:Ce3+, Tb3+may be promising tuning emission phosphor for white LEDs.
Sm3+, Eu3+or Sm3+/Eu3+doped Ca2BO3Cl phosphor can be excited by the long ultraviolet radiation excitation. Ca2BO3Cl:Sm3+can produce orange-red light (603nm) under401nm radiation excitation. Ca2BO3Cl:Eu3+can show red light (623nm) under392nm radiation excitation, however, it has a low absorption in the region of395-405nm. The emission intensity of Eu3+in Ca2BO3Cl can be enhanced by codoping Sm3+as a sensitizer, and the energy transfer efficiency (Sm3+→Eu3+) gradually increases to55%by increasing Eu3+doping content. It is found to be efficient to extend and strengthen the absorption of near-ultraviolet light in the region of395-405nm by codoping Sm3+. Moreover, the chromaticity coordinates of Ca2BO3Cl:Sm3+, Eu3+can also be influenced by the molar concentration of Eu3+, and the emission intensity and CIE can be compared to those of the conventional red phosphor Y2O2S:Eu3+. The result show Ca2BO3Cl:Sm3+, Eu3+may be promising red emitting phosphor for white LEDs.
Ca2BO3Cl:Tb3+and Ca2BO3Cl:Tb3+, A+(A=Li, Na, K) phopshors are prepared, and their luminescent properties are investigated.The emission intensity of Ca2BO3Cl:Tb3+can be enhanced about1.61,1.97and1.81times by codoping compersation charge Li+, Na+and K+, respectively, and the CIE chromaticity coordinates of Ca2BO3Cl:Tb3+, A+(A=Li,Na, K) are (0.335,0.584),(0.335,0.585) and (0.335,0.585), respectively. Hence, A+(A=Li, Na, K) may be the optimal charge compensator for Ca2BO3Cl:Tb3+, and Na+has the optimal effect.
引文
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