CN101368100B - Fluorescent powder transmitting yellow light and method of producing the same - Google Patents
Fluorescent powder transmitting yellow light and method of producing the same Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims abstract description 16
- 229910016036 BaF 2 Inorganic materials 0.000 claims abstract description 12
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 12
- 239000010431 corundum Substances 0.000 claims abstract description 12
- 239000000126 substance Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 230000004907 flux Effects 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 3
- 238000009877 rendering Methods 0.000 abstract description 3
- 238000005286 illumination Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 description 7
- 239000012856 weighed raw material Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 3
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 2
- 229910019990 cerium-doped yttrium aluminum garnet Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005090 crystal field Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
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Abstract
本发明涉及用于照明与显示技术领域的LED中的荧光粉，特别是一种用于制作白光LED的发射黄色光的荧光粉及其制备方法。是具有下述通式：Y3-x-yPbxCeyAl5O12，式中x＝0.01～0.10；y＝0.003～0.2。制备方法是：按化学式中各物质的化学计量比分别称取Y2O3、Al2O3、CeO2、和PbO，以BaF2作为助熔剂，一起研磨混合后，放入刚玉坩埚置于高温炉中，还原气氛下，加热至1300℃-1700℃，恒温3-7小时，自然冷却，即得本发明荧光粉。与Y3Al5O12:Ce荧光粉相比，有发光增强、发射峰位置红移的优点，用该材料制备的LED显色指数有所提高。The invention relates to a fluorescent powder used in LEDs in the technical field of illumination and display, in particular to a fluorescent powder emitting yellow light for making white LEDs and a preparation method thereof. It has the following general formula: Y 3-xy Pb x Ce y Al 5 O 12 , where x=0.01~0.10; y=0.003~0.2. The preparation method is: weigh Y 2 O 3 , Al 2 O 3 , CeO 2 , and PbO respectively according to the stoichiometric ratio of each substance in the chemical formula, use BaF 2 as a flux, grind and mix them together, put them into a corundum crucible and place In a high-temperature furnace, under a reducing atmosphere, heat to 1300°C-1700°C, keep the temperature constant for 3-7 hours, and cool naturally to obtain the phosphor powder of the present invention. Compared with Y 3 Al 5 O 12 :Ce phosphor, it has the advantages of enhanced luminescence and red-shifted emission peak position, and the color rendering index of LED prepared with this material is improved.
Description
技术领域technical field
本发明涉及用于照明与显示技术领域的发光二极管(LED)中的荧光粉，特别是一种用于制作白光LED的发射黄色光的荧光粉及其制备方法。The invention relates to phosphor powder used in light-emitting diodes (LEDs) in the technical field of illumination and display, in particular to phosphor powder emitting yellow light for making white LEDs and a preparation method thereof.
背景技术Background technique
白光发光二极管(LED)被普遍认为是21世纪替代传统照明器件的新光源。产生白光的方案主要采用在GaN蓝光LED芯片上涂敷发射黄色光的荧光粉。目前，黄色荧光粉主要以Y3Al5O12(YAG):Ce为主，该种荧光粉缺少红光成分使得所制备的LED显色指数偏低，因此，开发研制更为高效的发射黄色光的荧光粉将有效提高白光发光二极管(LED)的制作技术水平。White light-emitting diodes (LEDs) are generally considered to be a new light source to replace traditional lighting devices in the 21st century. The scheme of producing white light mainly adopts the phosphor powder that emits yellow light to be coated on the GaN blue light LED chip. At present, the yellow phosphor is mainly composed of Y 3 Al 5 O 12 (YAG):Ce. The lack of red light component of this kind of phosphor makes the color rendering index of the prepared LED low. Therefore, it is necessary to develop more efficient yellow emission Light-emitting phosphors will effectively improve the production technology level of white light-emitting diodes (LEDs).
发明内容Contents of the invention
本发明的目的是提出一种用于制作白光发光二极管(LED)的发射黄色光的荧光粉，以克服目前用于制作白光LED的黄色荧光材料存在的上述缺点，提高白光LED的质量水平。The object of the present invention is to propose a phosphor powder emitting yellow light for making white light-emitting diodes (LEDs), to overcome the above-mentioned shortcomings of yellow fluorescent materials currently used for making white light LEDs, and improve the quality level of white light LEDs.
本发明发射黄色光的荧光粉，是具有下述通式：Y3-x-yPbxCeyAl5O12，式中x＝0.01～0.10；y＝0.003～0.2。The fluorescent powder emitting yellow light of the present invention has the following general formula: Y 3-xy Pb x Ce y Al 5 O 12 , where x=0.01-0.10; y=0.003-0.2.
该荧光粉的组成特征是在YAG:Ce中引入Pb离子取代部分Y离子。因为Pb的离子半径大于Y3+，Pb的引入引起晶格畸变，晶格常数变大，晶体场劈裂变大，引起荧光粉的发光增强，同时，发射峰位置红移。The characteristic of the composition of the phosphor is that Pb ions are introduced into YAG:Ce to replace part of Y ions. Because the ionic radius of Pb is larger than that of Y 3+ , the introduction of Pb causes lattice distortion, the lattice constant increases, and the crystal field splitting increases, which causes the luminescence of the phosphor to be enhanced, and at the same time, the position of the emission peak is red-shifted.
该化合物中的Pb以等量的二价和四价离子存在，因此平均价态为三价。当Pb含量x＝0.05时，荧光粉的发光最强，比不加Pb的提高了大约10％，发射峰位置红移3nm左右。与Y3Al5O12(YAG):Ce荧光粉相比，有发光增强、 发射峰位置红移的优点，用该材料制备的LED显色指数有所提高。Pb in this compound exists in equal amounts of divalent and tetravalent ions, so the average valence state is trivalent. When the Pb content x=0.05, the luminescence of the phosphor is the strongest, which is about 10% higher than that without adding Pb, and the position of the emission peak is red-shifted by about 3nm. Compared with Y 3 Al 5 O 12 (YAG):Ce phosphor, it has the advantages of enhanced luminescence and red-shifted emission peak position, and the color rendering index of LED prepared with this material is improved.
本发明发射黄色光的荧光粉的制备方法包括以下步骤：The preparation method of the fluorescent powder emitting yellow light of the present invention comprises the following steps:
a.以Y2O3、Al2O3、CeO2、PbO为原料，按化学式Y3-x-y PbxCeyAl5O12中各元素的化学计量比分别称取计算量的粉体Y2O3、Al2O3、CeO2、PbO；a. Using Y 2 O 3 , Al 2 O 3 , CeO 2 , and PbO as raw materials, weigh the calculated amount of powder Y according to the stoichiometric ratio of each element in the chemical formula Y 3-xy Pb x Ce y Al 5 O 12 2 O 3 , Al 2 O 3 , CeO 2 , PbO;
b.将作为助熔剂的BaF2和步骤a称取的Y2O3、Al2O3、CeO2、PbO一起研磨混合均匀后放入刚玉坩埚中；b. Grind and mix BaF 2 as a flux with Y 2 O 3 , Al 2 O 3 , CeO 2 , and PbO weighed in step a and put them into a corundum crucible;
c.将步骤b所述装有混合料的刚玉坩埚置于高温炉中，在还原气氛下，加热至1300-1700℃，恒温3-7小时，自然冷却，取出即得所述的发射黄色光的荧光粉。c. Place the corundum crucible with the mixture in step b in a high-temperature furnace, heat it to 1300-1700°C in a reducing atmosphere, keep the temperature at a constant temperature for 3-7 hours, cool it naturally, and take it out to get the yellow light emitting of fluorescent powder.
所述的助熔剂BaF2的加入量为Y2O3、Al2O3、CeO2、PbO质量和的3％～5％。The added amount of the flux BaF 2 is 3%-5% of the mass sum of Y 2 O 3 , Al 2 O 3 , CeO 2 , and PbO.
附图说明Description of drawings
图1是本发明荧光粉发射强度随Pb浓度变化的曲线图。Fig. 1 is a graph showing the variation of the emission intensity of the phosphor powder of the present invention with the concentration of Pb.
具体实施方式Detailed ways
通过以下实施例对本发明作进一步详细说明。The present invention is further described in detail through the following examples.
实施例1Example 1
制备化学式为Y2.93Pb0.01Ce0.06Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.93 Pb 0.01 Ce 0.06 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.3081g Y2O3，2.5491g Al2O3，0.1033gCeO2，0.0223g PbO，再称取0.1794g BaF2作助溶剂；将称取的原料充分研磨混合均匀后，置入高纯刚玉坩埚，放入高温炉中；在CO或H2和N2还原气氛条件下，在1500℃加热3小时即得到黄光荧光粉Y2.93Pb0.01Ce0.06Al5O12。Weigh 3.3081g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.1033g CeO 2 , 0.0223g PbO according to the stoichiometric ratio of elements in the above formula, and then weigh 0.1794g BaF 2 as auxiliary solvent; fully grind the weighed raw materials After mixing evenly, put it into a high-purity corundum crucible and put it into a high-temperature furnace; under the condition of CO or H 2 and N 2 reducing atmosphere, heat at 1500°C for 3 hours to obtain yellow phosphor Y 2.93 Pb 0.01 Ce 0.06 Al 5 O 12 .
实施例2Example 2
制备化学式为Y2.89Pb0.05Ce0.06Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.89 Pb 0.05 Ce 0.06 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.2630g Y2O3，2.5491g Al2O3，0.1033gCeO2，0.1115g PbO，再称取0.1808g BaF2作助溶剂；将称取的原料充分研磨 混合均匀后，置入高纯刚玉坩埚，放入高温炉中；在CO或H2和N2还原气氛条件下，在1500℃加热3小时即得到黄光荧光粉Y2.89Pb0.05Ce0.06Al5O12。Weigh 3.2630g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.1033g CeO 2 , 0.1115g PbO according to the stoichiometric ratio of elements in the above formula, and then weigh 0.1808g BaF 2 as auxiliary solvent; fully grind the weighed raw materials After mixing evenly, put it into a high-purity corundum crucible and put it into a high-temperature furnace; under the condition of CO or H 2 and N 2 reducing atmosphere, heat at 1500°C for 3 hours to obtain yellow phosphor Y 2.89 Pb 0.05 Ce 0.06 Al 5 O 12 .
实施例3Example 3
制备化学式为Y2.84Pb0.1Ce0.06Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.84 Pb 0.1 Ce 0.06 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.2065g Y2O3，2.5491g Al2O3，0.1033gCeO2，0.2230g PbO，再称取0.1825g BaF2作助溶剂；将称取的原料充分研磨混合均匀后，置入高纯刚玉坩埚，放入高温炉中；在CO或H2和N2还原气氛条件下，在1500℃加热3小时即得到黄光荧光粉Y2.84Pb0.1Ce0.06Al5O12。Weigh 3.2065g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.1033g CeO 2 , 0.2230g PbO according to the stoichiometric ratio of elements in the above formula, and then weigh 0.1825g BaF 2 as auxiliary solvent; fully grind the weighed raw materials After mixing evenly, put it into a high-purity corundum crucible and put it into a high-temperature furnace; under the condition of CO or H 2 and N 2 reducing atmosphere, heat at 1500°C for 3 hours to obtain yellow phosphor Y 2.84 Pb 0.1 Ce 0.06 Al 5 O 12 .
实施例4Example 4
制备化学式为Y2.85Pb0.05Ce0.1Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.85 Pb 0.05 Ce 0.1 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.1839g Y2O3，2.5491g Al2O3，0.1721gCeO2，0.3230g PbO，0.1799g BaF2作助溶剂；将称取的原料充分研磨混合均匀后，置入高纯刚玉坩埚，放入高温炉中；在CO或H2和N2还原气氛条件下，在1500℃加热3小时即得到黄光荧光粉Y2.85Pb0.05Ce0.1Al5O12。Weigh 3.1839g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.1721g CeO 2 , 0.3230g PbO, 0.1799g BaF 2 as auxiliary solvent according to the stoichiometric ratio of elements in the above formula; fully grind and mix the weighed raw materials , placed in a high-purity corundum crucible, and placed in a high-temperature furnace; under CO or H 2 and N 2 reducing atmosphere conditions, heated at 1500°C for 3 hours to obtain yellow phosphor Y 2.85 Pb 0.05 Ce 0.1 Al 5 O 12 .
实施例5Example 5
制备化学式为Y2.8Pb0.05Ce0.15Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.8 Pb 0.05 Ce 0.15 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.2178g Y2O3，2.5491g Al2O3，0.2582gCeO2，0.1115g PbO，0.1841g BaF2作助溶剂；将称取的原料充分研磨混合均匀后，置入高纯刚玉坩埚，放入高温炉中；在CO或H2和N2还原气氛条件下，在1500℃加热3小时即得到黄光荧光粉Y2.8Pb0.05Ce0.15Al5O12。Weigh 3.2178g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.2582g CeO 2 , 0.1115g PbO, 0.1841g BaF 2 as auxiliary solvent according to the stoichiometric ratio of elements in the above formula; , placed in a high-purity corundum crucible, and placed in a high-temperature furnace; under CO or H 2 and N 2 reducing atmosphere conditions, heated at 1500°C for 3 hours to obtain yellow phosphor Y 2.8 Pb 0.05 Ce 0.15 Al 5 O 12 .
实施例6Example 6
制备化学式为Y2.947Pb0.05Ce0.003Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.947 Pb 0.05 Ce 0.003 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.3273g Y2O3，2.5491g Al2O3，0.0053gCeO2，0.1115g PbO，0.1798g BaF2作助溶剂；将称取的原料充分研磨混合均匀后，置入高纯刚玉坩埚，放入高温炉中；在CO或H2和N2还原气氛条 件下，在1500℃加热3小时即得到黄光荧光粉Y2.947Pb0.05Ce0.003Al5O12。Weigh 3.3273g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.0053g CeO 2 , 0.1115g PbO, 0.1798g BaF 2 as auxiliary solvent according to the stoichiometric ratio of elements in the above formula; fully grind and mix the weighed raw materials , placed in a high-purity corundum crucible, and placed in a high-temperature furnace; under CO or H 2 and N 2 reducing atmosphere conditions, heated at 1500°C for 3 hours to obtain yellow phosphor Y 2.947 Pb 0.05 Ce 0.003 Al 5 O 12 .
实施例7Example 7
制备化学式为Y2.75Pb0.05Ce0.2Al5O12的黄光荧光粉。A yellow fluorescent powder with a chemical formula of Y 2.75 Pb 0.05 Ce 0.2 Al 5 O 12 was prepared.
按上式中元素化学计量比称取3.1420g Y2O3，2.5491g Al2O3，0.3442gCeO2，0.1115g PbO，0.1844g BaF2作助溶剂；将称取的原料充分研磨混合均匀后，置入高纯刚玉坩埚，放入高温炉中。在CO或H2和N2还原气氛条件下，在1500℃加热3小时即得到黄光荧光粉Y2.75Pb0.05Ce0.2Al5O12。Weigh 3.1420g Y 2 O 3 , 2.5491g Al 2 O 3 , 0.3442g CeO 2 , 0.1115g PbO, 0.1844g BaF 2 as auxiliary solvent according to the stoichiometric ratio of elements in the above formula; , placed in a high-purity corundum crucible, and placed in a high-temperature furnace. Under the reducing atmosphere of CO or H 2 and N 2 , heating at 1500° C. for 3 hours can obtain the yellow phosphor Y 2.75 Pb 0.05 Ce 0.2 Al 5 O 12 .
荧光粉的发光强度随着Pb含量x的变化而变化，如图1所示，当Pb含量x＝0.05时，荧光粉的发光强度最高。The luminous intensity of the phosphor varies with the change of the Pb content x, as shown in FIG. 1 , when the Pb content x=0.05, the luminous intensity of the phosphor is the highest.
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| 李长敏.LED暖白光照明用(Y2.95-xGdxCe0.05)Al5O12系列荧光粉的晶相与三维荧光光谱.《大连轻工业学院学报》.2007,第26卷(第2期),全文. * |
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