CN106520117A - A kind of preparation method of LiLa(MoO4)2:Eu3+ fluorescent powder - Google Patents
A kind of preparation method of LiLa(MoO4)2:Eu3+ fluorescent powder Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 26
- 229910015667 MoO4 Inorganic materials 0.000 title claims abstract 4
- 238000002360 preparation method Methods 0.000 title claims description 17
- 238000003746 solid phase reaction Methods 0.000 claims abstract description 13
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract 7
- 239000000463 material Substances 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 13
- 239000000376 reactant Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010671 solid-state reaction Methods 0.000 claims 4
- RSEIMSPAXMNYFJ-UHFFFAOYSA-N europium(III) oxide Inorganic materials O=[Eu]O[Eu]=O RSEIMSPAXMNYFJ-UHFFFAOYSA-N 0.000 claims 3
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims 3
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims 3
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims 2
- 229910052808 lithium carbonate Inorganic materials 0.000 claims 2
- 238000010792 warming Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 20
- 239000002994 raw material Substances 0.000 abstract description 20
- 238000000034 method Methods 0.000 abstract description 15
- 239000000126 substance Substances 0.000 abstract description 8
- 239000007795 chemical reaction product Substances 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000005215 recombination Methods 0.000 abstract 1
- 230000006798 recombination Effects 0.000 abstract 1
- 239000007790 solid phase Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 17
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 15
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 8
- 238000000295 emission spectrum Methods 0.000 description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 description 5
- 238000003980 solgel method Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000012190 activator Substances 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000003836 solid-state method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7728—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals containing europium
- C09K11/7736—Vanadates; Chromates; Molybdates; Tungstates
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Abstract
Description
【技术领域】【Technical field】
本发明涉及荧光粉制备领域，具体涉及一种LiLa(MoO4)2:Eu3+荧光粉的制备方法。The invention relates to the field of phosphor preparation, in particular to a preparation method of LiLa(MoO 4 ) 2 :Eu 3+ phosphor.
【背景技术】【Background technique】
大多数的无机发光材料是由基质和激活剂组成。基质是发光材料的主体化合物，是由具有一定晶体结构稳定的晶体充当。激活剂的量很少，在材料中部分取代基质晶体中原有格位上的离子，形成杂质缺陷。Most phosphors are composed of a host and an activator. The matrix is the host compound of the luminescent material, which is acted by a stable crystal with a certain crystal structure. The amount of the activator is very small, and partially replaces the ions on the original site in the matrix crystal in the material, forming impurity defects.
充当基质的材料有很多种，其中具有白钨矿结构的双钼酸盐和双钨酸盐受到了人们的广泛关注，该类化合物的物理、化学性质稳定。在双钼酸盐的大家族中，LiLa(MoO4)2属于四方相。制备无机发光材料的方法有很多种，例如高温固相法、溶胶凝胶法、水热法和共沉淀法等等，与水热法等传统的湿化学法相比，高温固相法具有污染小(不使用酸或碱)、操作简单、产量大等优点，而被广泛应用于工业生产和实验研究中。目前对于以LiLa(MoO4)2为基质的发光材料的研究较少，Jinsheng Liao等人用溶胶凝胶法制备了LiLa(MoO4)2:Eu3+荧光粉，研究了其发光性能(Optical Materials，2012,8(34)，1468)；但溶胶凝胶法所使用的原料较贵，有些原料为有机物，对健康有害，并且制备时间较长，常需要几天或几周时间。然而，目前，还没有关于固相法制备LiLa(MoO4)2:Eu3+荧光粉的报道。There are many kinds of materials used as matrix, among which the double molybdate and double tungstate with scheelite structure have received widespread attention, and these compounds have stable physical and chemical properties. In the large family of double molybdates, LiLa(MoO 4 ) 2 belongs to the tetragonal phase. There are many methods for preparing phosphors, such as high-temperature solid-phase method, sol-gel method, hydrothermal method and co-precipitation method, etc. Compared with traditional wet chemical methods such as hydrothermal method, high-temperature solid-phase method has less pollution (do not use acid or alkali), simple operation, large output and other advantages, and are widely used in industrial production and experimental research. At present, there are few studies on luminescent materials based on LiLa(MoO 4 ) 2 . Jinsheng Liao et al. prepared LiLa(MoO 4 ) 2 :Eu 3+ phosphors by sol-gel method, and studied its luminescent properties (Optical Materials, 2012, 8(34), 1468); however, the raw materials used in the sol-gel method are more expensive, and some raw materials are organic matter, which is harmful to health, and the preparation time is longer, often requiring days or weeks. However, at present, there is no report on the preparation of LiLa(MoO 4 ) 2 :Eu 3+ phosphor by solid-state method.
【发明内容】【Content of invention】
本发明的目的在于提供一种LiLa(MoO4)2:Eu3+荧光粉的制备方法，此制备方法具有操作简单，产物结晶度高优点。The purpose of the present invention is to provide a preparation method of LiLa(MoO 4 ) 2 :Eu 3+ phosphor, which has the advantages of simple operation and high crystallinity of the product.
为了达到上述目的，本发明采用如下技术方案：In order to achieve the above object, the present invention adopts following technical scheme:
包括以下步骤：Include the following steps:
(1)称取Li2CO3、La2O3、MoO3以及Eu2O3粉体并混合均匀，得到反应物原料；其中Li2CO3、La2O3、MoO3和Eu2O3的摩尔比为1：(1-x)：4：x，x＝0.01～0.21；(1) Weigh Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders and mix them uniformly to obtain reactant raw materials; where Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O The molar ratio of 3 is 1:(1-x):4:x, x=0.01～0.21;
(2)反应物原料在600～1000℃进行固相反应，得到反应产物；(2) The raw material of the reactant is subjected to a solid phase reaction at 600-1000° C. to obtain a reaction product;
(3)反应产物冷却至室温后经过研磨，得到LiLa(MoO4)2:Eu3+荧光粉。(3) The reaction product is cooled to room temperature and ground to obtain LiLa(MoO 4 ) 2 :Eu 3+ phosphor.
进一步地，x＝0.17。Further, x=0.17.
进一步地，步骤(1)中的Li2CO3、La2O3、MoO3以及Eu2O3粉体是通过搅拌10～30min混合均匀的。Further, the Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders in the step (1) are uniformly mixed by stirring for 10-30 minutes.
进一步地，步骤(2)中反应物原料装在坩埚中，将装有反应物原料的坩埚放入马弗炉中进行固相反应。Further, in the step (2), the reactant raw material is packed in a crucible, and the crucible containing the reactant raw material is put into a muffle furnace for solid phase reaction.
进一步地，步骤(2)中采用120℃/min的升温速率升温至600～1000℃。Further, in step (2), the temperature is raised to 600-1000° C. at a heating rate of 120° C./min.
进一步地，步骤(2)中固相反应的时间为4～5h。Further, the solid-phase reaction time in step (2) is 4-5 hours.
进一步地，步骤(2)中固相反应的温度为800℃。Further, the temperature of the solid phase reaction in step (2) is 800°C.
进一步地，步骤(3)中研磨半小时。Further, grind for half an hour in step (3).
与现有技术相比，本发明具有以下有益的技术效果：Compared with the prior art, the present invention has the following beneficial technical effects:
本发明采用高温固相法，首先按照化学计量比称取Li2CO3、La2O3、MoO3和Eu2O3粉体，并将其混合搅拌均匀，进行高温反应，利用在高温的条件下反应原料化学键的断裂和重新组合，从而形成纯相结构的LiLa(MoO4)2:Eu3+荧光粉。本发明原料来源较广，成本较低，不含有毒有机物；本发明制得的荧光粉能够被蓝光有效激发，并发射出主峰位于618nm的红光。与现有的湿化学法相比，本发明的制备工艺简单，污染小、产量大，适用于大规模工业生产，易于商业化。The present invention adopts a high-temperature solid-phase method. First, Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders are weighed according to the stoichiometric ratio, mixed and stirred evenly, and subjected to a high-temperature reaction. The chemical bonds of the reaction materials are broken and recombined under the conditions, thereby forming the LiLa(MoO 4 ) 2 :Eu 3+ phosphor with a pure phase structure. The invention has wide sources of raw materials, low cost and no toxic organic matter; the phosphor powder prepared by the invention can be effectively excited by blue light and emit red light with a main peak at 618nm. Compared with the existing wet chemical method, the preparation process of the present invention is simple, with little pollution and large output, suitable for large-scale industrial production and easy to commercialize.
进一步地，本发明中固相反应的时间为4～5h，反应时间短，较溶胶凝胶法有效提高效率。Further, the time of the solid-phase reaction in the present invention is 4-5 hours, the reaction time is short, and the efficiency is effectively improved compared with the sol-gel method.
【附图说明】【Description of drawings】
图1是本发明所制备的LiLa(MoO4)2:Eu3+粉体的XRD图谱；Fig. 1 is the XRD pattern of LiLa(MoO 4 ) 2 :Eu 3+ powder prepared in the present invention;
图2是在不同反应温度下制备的LiLa(MoO4)2:Eu3+粉体的发射光谱；Figure 2 is the emission spectra of LiLa(MoO 4 ) 2 :Eu 3+ powders prepared at different reaction temperatures;
图3是在不同掺杂浓度下制备的LiLa(MoO4)2:Eu3+粉体的发射光谱。Fig. 3 is the emission spectrum of LiLa(MoO 4 ) 2 :Eu 3+ powder prepared under different doping concentrations.
【具体实施方式】【detailed description】
下面结合附图，对本发明作详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings.
本发明包括如下步骤：The present invention comprises the steps:
(1)用电子天平称取定量的Li2CO3，La2O3,MoO3以及Eu2O3粉体；其中Li2CO3、La2O3、MoO3和Eu2O3的摩尔比为1：(1-x)：4：x，x＝0.01～0.21；(1) Weigh quantitative Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders with an electronic balance; the moles of Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 The ratio is 1:(1-x):4:x, x=0.01～0.21;
(2)将称取的反应物粉体搅拌10～30min使其充分混合均匀；(2) Stir the weighed reactant powder for 10-30 minutes to fully mix it;
(3)将混合均匀的反应物原料倒入坩埚；(3) Pour the uniformly mixed reactant raw materials into the crucible;
(4)将坩埚放入马弗炉中进行反应，升温速率为120℃/min，当温度上升到指定温度后保温时间为4～5h，固相反应的温度为600～1000℃；(4) Put the crucible into the muffle furnace for reaction, the heating rate is 120°C/min, when the temperature rises to the specified temperature, the holding time is 4-5h, and the temperature of the solid phase reaction is 600-1000°C;
(5)固相反应结束后，待坩埚自然冷却至室温，将产物刮出，研磨半小时后成粉体，即得目标产物。(5) After the solid-phase reaction is completed, the crucible is naturally cooled to room temperature, the product is scraped off, ground for half an hour, and then powdered to obtain the target product.
以下通过具体的实施例对本发明做进一步详细说明。The present invention will be described in further detail below through specific examples.
实施例1：Example 1:
(1)采用Li2CO3，La2O3,MoO3以及Eu2O3粉体作为原料，其中Li2CO3、La2O3、MoO3和Eu2O3的摩尔比为1：(1-x)：4：x，x＝0.07mol；将上述原料搅拌10min使其充分混合均匀；(1) Use Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders as raw materials, where the molar ratio of Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 is 1: (1-x): 4: x, x=0.07mol; Stir the above raw materials for 10 minutes to fully mix them;
(2)将混合物倒入坩埚中；(2) Pour the mixture into the crucible;
(3)将坩埚放入马弗炉中，设定升温速率为120℃/min，反应温度分别设置为600℃，700℃，800℃，900℃以及1000℃，保温时间为4h，；(3) Put the crucible into the muffle furnace, set the heating rate to 120°C/min, set the reaction temperature to 600°C, 700°C, 800°C, 900°C and 1000°C respectively, and set the holding time to 4h;
(4)产物中Eu3+的掺杂浓度固定在7mol.％；(4) The doping concentration of Eu 3+ in the product is fixed at 7mol.%;
(5)固相反应结束后，待坩埚自然冷却至室温，将产物刮出，研磨成粉体，即得目标产物。(5) After the solid phase reaction is completed, the crucible is naturally cooled to room temperature, the product is scraped off, and ground into powder to obtain the target product.
图1为利用本发明实施例1所述方法制备的样品的XRD衍射图谱，从图中可以看出：当反应温度为600℃时，所制备的样品中含有MoO3·2H2O的杂峰，当反应温度升高到700℃，800℃，900℃和1000℃时，所制备样品的所有衍射峰位置均与四方相LiLa(MoO4)2的标准衍射图谱(JCPDS Card 18-0734)相吻合，表明所制备的样品均为纯相物质。Figure 1 is the XRD diffraction pattern of the sample prepared by the method described in Example 1 of the present invention. It can be seen from the figure that when the reaction temperature is 600°C, the prepared sample contains the miscellaneous peak of MoO 3 ·2H 2 O , when the reaction temperature increased to 700°C, 800°C, 900°C and 1000°C, all the diffraction peak positions of the prepared samples were consistent with the standard diffraction pattern (JCPDS Card 18-0734) of tetragonal LiLa(MoO 4 ) 2 It is consistent, indicating that the prepared samples are all phase-pure substances.
图2为利用本发明实施例1所述方法制备样品的发射光谱，激发波长为465nm。从图中可以看出：在不同反应温度的条件下制备样品的发射光谱形状相似，而发光强度不同，其中800℃条件下制备的样品发光强度最强，当用465nm的光激发时，能够观测到Eu3+的5D0→7F1和5D0→7F2的跃迁峰，其中主峰位于618nm。Fig. 2 is the emission spectrum of the sample prepared by the method described in Example 1 of the present invention, and the excitation wavelength is 465nm. It can be seen from the figure that the emission spectra of the samples prepared at different reaction temperatures are similar in shape, but the luminous intensity is different. Among them, the luminous intensity of the sample prepared at 800 ° C is the strongest. When excited with 465nm light, it can be observed The transition peaks of 5 D 0 → 7 F 1 and 5 D 0 → 7 F 2 to Eu 3+ , where the main peak is located at 618nm.
实施例2：Example 2:
(1)采用Li2CO3，La2O3,MoO3以及Eu2O3粉体作为原料，其中Li2CO3、La2O3、MoO3和Eu2O3的摩尔比为1：(1-x)：4：x，x＝0.01mol、0.05mol、0.09mol、0.13mol、0.17mol以及0.21mol；将上述原料搅拌10min使其充分混合均匀；(1) Use Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders as raw materials, where the molar ratio of Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 is 1: (1-x): 4: x, x=0.01mol, 0.05mol, 0.09mol, 0.13mol, 0.17mol and 0.21mol; stir the above raw materials for 10 minutes to make them fully mixed;
(2)将混合物倒入坩埚中；(2) Pour the mixture into the crucible;
(3)将坩埚放入马弗炉中，设定升温速率为120℃/min，反应温度设置为800℃；保温时间为4h；(3) Put the crucible into the muffle furnace, set the heating rate to 120°C/min, and set the reaction temperature to 800°C; the holding time is 4h;
(4)产物中Eu3+的掺杂浓度分别为1mol.％,5mol.％,9mol.％,13mol.％,17mol.％,21mol.％；(4) The doping concentration of Eu 3+ in the product is 1mol.%, 5mol.%, 9mol.%, 13mol.%, 17mol.%, 21mol.%, respectively;
(5)反应结束后，待坩埚自然冷却至室温，将产物研磨成粉体，即得目标产物。(5) After the reaction, the crucible is naturally cooled to room temperature, and the product is ground into powder to obtain the target product.
图3为利用本发明实施例2所述方法制备的样品的发射光谱，激发波长为465nm。从图中可以看出：在不同掺杂浓度条件下样品的发射光谱相似，而发光强度不同，当Eu3+的掺杂浓度从1mol.％增加到17mol.％时，样品的发光强度随着掺杂浓度的升高而增强，当Eu3+的掺杂浓度超过17mol.％后，样品的发光强度随着掺杂浓度的升高而下降，在高于21mol％后出现浓度淬灭现象，因此，Eu3+的最佳掺杂浓度为17mol.％。Fig. 3 is the emission spectrum of the sample prepared by the method described in Example 2 of the present invention, and the excitation wavelength is 465nm. It can be seen from the figure that the emission spectra of the samples are similar under different doping concentration conditions, but the luminous intensity is different. When the doping concentration of Eu 3+ increases from 1mol.% to 17mol.%, the luminous intensity of the sample increases with When the doping concentration of Eu 3+ is higher than 17mol.%, the luminescence intensity of the sample decreases with the increase of doping concentration, and the concentration quenching phenomenon occurs when the doping concentration is higher than 21mol%. Therefore, the optimum doping concentration of Eu 3+ is 17mol.%.
实施例三Embodiment Three
(1)采用Li2CO3，La2O3,MoO3以及Eu2O3粉体作为原料，其中Li2CO3、La2O3、MoO3和Eu2O3的摩尔比为1：(1-x)：4：x，x＝0.04mol；将上述原料搅拌20min使其充分混合均匀；(1) Use Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders as raw materials, where the molar ratio of Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 is 1: (1-x): 4: x, x=0.04mol; Stir the above raw materials for 20 minutes to fully mix them;
(2)将混合物倒入坩埚中；(2) Pour the mixture into the crucible;
(3)将坩埚放入马弗炉中，设定升温速率为120℃/min，反应温度设置为800℃，保温时间分别为3h、4h、4.5h、5h和6h；(3) Put the crucible into the muffle furnace, set the heating rate to 120°C/min, set the reaction temperature to 800°C, and set the holding time to 3h, 4h, 4.5h, 5h and 6h respectively;
(4)产物中Eu3+的掺杂浓度分别为4mol.％；(4) The doping concentration of Eu 3+ in the product is 4mol.% respectively;
(5)反应结束后，待坩埚自然冷却至室温，将产物研磨成粉体，即得目标产物。(5) After the reaction, the crucible is naturally cooled to room temperature, and the product is ground into powder to obtain the target product.
经过测试发现，本发明中保温时间低于4h时目标产物出现杂相，时间太长会消耗较高能量，最佳为4h。After testing, it is found that in the present invention, when the holding time is lower than 4h, the target product has an impurity phase, and if the time is too long, high energy will be consumed, and the optimum time is 4h.
实施例四Embodiment four
(1)采用Li2CO3，La2O3,MoO3以及Eu2O3粉体作为原料，其中Li2CO3、La2O3、MoO3和Eu2O3的摩尔比为1：(1-x)：4：x，x＝0.08mol；将上述原料搅拌30min使其充分混合均匀；(1) Use Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders as raw materials, where the molar ratio of Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 is 1: (1-x): 4: x, x=0.08mol; Stir the above raw materials for 30 minutes to fully mix them;
(2)将混合物倒入坩埚中；(2) Pour the mixture into the crucible;
(3)将坩埚放入马弗炉中，设定升温速率为120℃/min，反应温度设置为850℃，保温时间分别为4h；(3) Put the crucible into the muffle furnace, set the heating rate to 120°C/min, set the reaction temperature to 850°C, and set the holding time to 4h;
(4)产物中Eu3+的掺杂浓度分别为8mol.％；(4) The doping concentration of Eu 3+ in the product is 8mol.% respectively;
(5)反应结束后，待坩埚自然冷却至室温，将产物研磨成粉体，即得目标产物。(5) After the reaction, the crucible is naturally cooled to room temperature, and the product is ground into powder to obtain the target product.
本发明公开了一种LiLa(MoO4)2:Eu3+荧光粉的制备方法和发光特性。本发明采用高温固相法，利用在高温的条件下反应原料化学键的断裂和重新组合，从而形成新物质。首先按照化学计量比称取Li2CO3、La2O3、MoO3和Eu2O3粉体，并将其混合搅拌均匀，将混合物倒入至坩埚，并将坩埚放在马弗炉中进行高温反应，待反应完成自然冷却至室温后；经粉碎、研磨得到目标产物。该荧光粉能够被蓝光有效激发，并发射出主峰位于618nm的红光。The invention discloses a preparation method and luminous characteristics of LiLa(MoO 4 ) 2 :Eu 3+ fluorescent powder. The invention adopts a high-temperature solid-phase method to form new substances by breaking and recombining chemical bonds of raw materials under high-temperature conditions. First, weigh Li 2 CO 3 , La 2 O 3 , MoO 3 and Eu 2 O 3 powders according to the stoichiometric ratio, mix and stir them evenly, pour the mixture into a crucible, and place the crucible in a muffle furnace Carry out high-temperature reaction, and after the reaction is completed, cool naturally to room temperature; obtain the target product by crushing and grinding. The phosphor can be effectively excited by blue light and emit red light with a main peak at 618nm.
本发明采用固相法，通过调节反应温度和Eu3+的掺杂浓度，研究这些因素对LiLa(MoO4)2:Eu3+样品的结构和发光性能的影响，对发光材料的制备和研究具有重要意义。The present invention adopts the solid phase method, by adjusting the reaction temperature and the doping concentration of Eu 3+ , to study the influence of these factors on the structure and luminescent properties of LiLa(MoO 4 ) 2 :Eu 3+ samples, and to the preparation and research of luminescent materials. is of great significance.
以上所述仅为本发明的较佳实施方式，不是唯一的实施方式，凡在本发明的精神和原则之内，在未背离本工艺过程下所做的任何修改，等同替换，改进等，均为本发明的权利要求所涵盖。The above is only a preferred embodiment of the present invention, not the only embodiment. Any modification, equivalent replacement, improvement, etc. within the spirit and principle of the present invention without departing from the process are all covered by the claims of the present invention.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107338052A (en) * | 2017-07-31 | 2017-11-10 | 陕西科技大学 | A kind of rear-earth-doped lanthanum molybdate lithium fluorescent material of tunable optical and preparation method thereof |
| CN107384397A (en) * | 2017-07-31 | 2017-11-24 | 陕西科技大学 | A kind of lanthanum molybdate lithium fluorescent material of dysprosium doped and preparation method thereof |
| CN110295044A (en) * | 2019-07-22 | 2019-10-01 | 通化师范学院 | A kind of very high rare earth Eu of luminous intensity3+Ion doping gadolinium molydbate lithium red fluorescence powder, preparation method thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU409962A1 (en) * | 1971-05-04 | 1974-01-05 | ||
| CN1462789A (en) * | 2003-05-21 | 2003-12-24 | 温州师范学院 | Red fluorescence powder |
| CN101358129A (en) * | 2007-08-03 | 2009-02-04 | 同济大学 | A kind of preparation method of red nano phosphor powder for LED |
| CN101519589A (en) * | 2009-03-27 | 2009-09-02 | 中国地质大学（武汉） | High-luminance finely ground particle red fluorescent powder and preparation method thereof |
| CN101717636A (en) * | 2009-11-16 | 2010-06-02 | 孙家跃 | Upconversion material and preparation method thereof |
| CN101781555A (en) * | 2009-01-16 | 2010-07-21 | 中国科学院福建物质结构研究所 | Deep red phosphor powder suitable to be excited by blue LED, preparation method thereof, and electric light source made by same |
| CN105038791A (en) * | 2015-06-23 | 2015-11-11 | 西安建筑科技大学 | Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light |
-
2016
- 2016-10-31 CN CN201610933200.1A patent/CN106520117A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU409962A1 (en) * | 1971-05-04 | 1974-01-05 | ||
| CN1462789A (en) * | 2003-05-21 | 2003-12-24 | 温州师范学院 | Red fluorescence powder |
| CN101358129A (en) * | 2007-08-03 | 2009-02-04 | 同济大学 | A kind of preparation method of red nano phosphor powder for LED |
| CN101781555A (en) * | 2009-01-16 | 2010-07-21 | 中国科学院福建物质结构研究所 | Deep red phosphor powder suitable to be excited by blue LED, preparation method thereof, and electric light source made by same |
| CN101519589A (en) * | 2009-03-27 | 2009-09-02 | 中国地质大学（武汉） | High-luminance finely ground particle red fluorescent powder and preparation method thereof |
| CN101717636A (en) * | 2009-11-16 | 2010-06-02 | 孙家跃 | Upconversion material and preparation method thereof |
| CN105038791A (en) * | 2015-06-23 | 2015-11-11 | 西安建筑科技大学 | Preparation method of spherical red phosphor powder capable of being excited by ultraviolet-blue light |
Non-Patent Citations (1)
| Title |
|---|
| HIYONG ZHANG等: "Synthesis and Luminescent Properties of Eu3+ Doped Double Molybdate Phosphors", 《ADVANCED MATERIALS RESEARCH》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107338052A (en) * | 2017-07-31 | 2017-11-10 | 陕西科技大学 | A kind of rear-earth-doped lanthanum molybdate lithium fluorescent material of tunable optical and preparation method thereof |
| CN107384397A (en) * | 2017-07-31 | 2017-11-24 | 陕西科技大学 | A kind of lanthanum molybdate lithium fluorescent material of dysprosium doped and preparation method thereof |
| CN110295044A (en) * | 2019-07-22 | 2019-10-01 | 通化师范学院 | A kind of very high rare earth Eu of luminous intensity3+Ion doping gadolinium molydbate lithium red fluorescence powder, preparation method thereof |
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