基于%5BLnMo_%2812%29%5D二十面体的三维稀土钼酸盐骨架的合成、结构及荧光性能%28英文%29.pdf
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1、第39卷第11期2023年11月Vol.39 No.1122092218无机化学学报CHINESE JOURNAL OF INORGANIC CHEMISTRY收稿日期:20230411。收修改稿日期:20230914。国家自然科学基金(No.21871262,21901242)、福建省自然科学基金(No.2020J05080)、厦门自然科学基金(No.3502Z20206080)、中国科学院重点研究计划(No.ZDRWCN202133)和中国科学院青年创新促进会(No.2021302)资助。通信联系人。Email:,基于LnMo12二十面体的三维稀土钼酸盐骨架的合成、结构及荧光性能黄敏1,2
2、,3,4卓著1,2,3陈婷1,2,3,4路自修,2,3王维,1,2,3,4黄有桂,1,2,3,4(1福建师范大学化学与材料学院,福州350002)(2中国科学院福建物质结构研究所,中国科学院功能纳米结构设计与组装重点实验室,福建省纳米材料重点实验室,福州350002)(3中国科学院海西研究院厦门稀土材料研究所,稀土光电功能材料厦门重点实验室,厦门361021)(4中国科学院大学福建学院,福州350002)摘要:通过缓慢蒸发溶剂法合成了2例新的三维稀土钼酸盐:Ln(H2O)33LnMo12O42xH2O,其中Ln=Eu(1)、Tb(2),x=7(1),10.17(2)。这2种稀土钼酸盐中都含有新
3、颖的二十面体LnMo12O42构建单元,该单元通过与LnO9多面体进一步连接形成三维网络。光致发光测试表明,化合物1和2显示出明显不同的发射特征,这与Eu3+和Tb3+离子的不同能级跃迁密切相关。化合物1表现出较强的红色发射(CIE色度坐标为(0.66,0.33)、高发光强度、较大的荧光量子产率(约60%),对应于从5D0到7FJ(J=4、3、2、1、0)的跃迁;化合物2表现出浅绿色发射(CIE色度坐标为(0.34,0.60),对应从5D4到7FJ(J=6、5、4、3)的能级跃迁,其发光强度较弱和荧光量子产率较低(约20%)。有趣的是,一定量的Tb3+引入和大量溶剂分子的存在导致化合物2发生部
4、分荧光猝灭,但对化合物1的荧光几乎没有影响。关键词:稀土钼酸盐;晶体结构;光致发光;荧光淬灭;配位化学;荧光粉中图分类号:O614.33+8;O614.341文献标识码:A文章编号:10014861(2023)11220910DOI:10.11862/CJIC.2023.176Synthesis,crystal structure,and luminescence properties of threedimensionalrare earth molybdate framework based on LnMo12 icosahedronHUANG Min1,2,3,4ZHUO Zhu1,2,
5、3CHEN Ting1,2,3,4LU ZiXiu,2,3WANG Wei,1,2,3,4HUANG YouGui,1,2,3,4(1College of Chemistry and Materials Science,Fujian Normal University,Fuzhou 350002,China)(2CAS Key Laboratory of Design and Assembly of Functional Nanostructures,Fujian Provincial Key Laboratory of Nanomaterials,Fujian Institute of Re
6、search on the Structure of Matter,Chinese Academy of Sciences,Fuzhou 350002,China)(3Xiamen Key Laboratory of Rare Earth Photoelectric Functional Materials,Xiamen Institute of Rare Earth Materials,Haixi Institutes,Chinese Academy of Sciences,Xiamen,Fujian 361021,China)(4Fujian College,University of C
7、hinese Academy of Sciences,Fuzhou 350002,China)Abstract:Two new 3D rareearth molybdate frameworks,Ln(H2O)33LnMo12O42xH2O,where Ln=Eu(1),Tb(2);x=7(1),10.17(2),have been synthesized by slow evaporation.Both of these rare earth molybdate frameworks have anew rareearthcentered icosahedron LnMo12O42 buil
8、ding unit,which is further connected to adjacent ones byLnO9 polyhedra to form a 3D network.Photoluminescence tests reveal that 1 and 2 exhibited different emissionproperties,which are caused by the forbital energy levels of Eu3+and Tb3+.1 exhibited bright red emissions(CIE无机化学学报第39卷chromaticity coo
9、rdinates:(0.66,0.33)corresponding to the transition from5D0to7FJ(J=4,3,2,1,0),with high luminescent emission intensity and high quantum yield(about 60%).2 exhibited light green emissions(CIE chromaticitycoordinates:(0.34,0.60)corresponding to the transition from5D4to7FJ(J=6,5,4,3),with lower lumines
10、cent emission intensity and quantum yield(about 20%).Interestingly,the introduction of Tb and the presence of a large number of solvent molecules in compound 2,both lead to partial fluorescence quenching but have little effect on the fluorescence properties of 1.CCDC:2254280,1;2254281,2.Keywords:rar
11、eearth molybdate;photoluminescence;crystal structure;fluorescence quenching;phosphor0IntroductionRareearth molybdates possess interesting structures because of the flexibility of coordination numberand geometry of both Ln3+and Mo6+ions15.The diversestructures of rare earth molybdates lead to unique
12、physical and chemical properties,such as magnetism,luminescence,and catalysis510.Among various properties,the photoluminescence properties of rareearth molybdates are of particular interest and have been widelyinvestigated.As we know,rareearth ions with rich energy levels,as the most popular activat
13、ors,enable luminescent emissions over the ultraviolet visible near infrared(UVVisNIR)spectral region via ff or dftransitions.The 4f orbitals of Ln3+ions are shielded bythe 5s25p6subshells and therefore give highly intensivenarrowband emissions,making them attractive for awide range of applications s
14、uch as displays,luminescent sensors,and medical probes for clinical use.Famous examples include the Eu3+and Tb3+based compounds with red(5D07FJtransition)and green(5D47FJtransition)luminescence,respectively.On the other hand,molybdates generally have goodchemical stability,thermal stability,luminesc
15、ent properties,mechanical properties,and thermal conductivity1113.The molybdate matrix also has a strong and widecharge absorption band in the near ultraviolet range.Under ultraviolet excitation,the energy is transferredto the active ions through nonradiative transitions.Bycombining rare earth ions
16、and Mo6+into rare earthmolybdates,excellent performance can be realized.Forexample,Ln2MoO6(Ln=rare earth)14,Ln2Mo2O915,Ln2Mo3O1216,Ln2Mo5O1817,Ln2Mo4O1518,Ln4Mo7O2719,Ln6MoO1220,Ln6Mo10O3921,Nb12.4MgMo13O3622,andLnEuMo2O823(A=alkali metal)were found to have different structural characteristics and f
17、luorescence performances.Up to now,the synthesis of new rareearthmolybdates with well designed structures is still animportant research topic.This is because the chemicaland physical properties of a material closely depend onits composition,structure,crystalline phase,shape,particle size,and dimensi
18、onality2427.It is therefore important to obtain new rare earth molybdates exhibitinggood luminescence performances,to explore the relationship between crystal structure and luminescenceperformance.In this work,two new 3D rare earth molybdateframeworks,Ln(H2O)33LnMo12O42xH2O,where Ln=Eu(1),Tb(2);x=7(
19、1),10.17(2),were synthesized forthe first time via a facile slow evaporation method.Thecrystal structures were determined and the luminescence properties were investigated.1Experimental1.1Starting materials and instrumentsAll chemicals,including Tb(NO3)36H2O(AdamasCo.,Ltd.,purity greater than 99.99%
20、),Eu(NO3)35H2O(AdamasCo.,Ltd.,puritygreaterthan99.99%),Co(NO3)26H2O(Adamas Co.,Ltd.,99%),thiodiglycolicacid(Bidepharm Co.,Ltd.,98%),and Na2MoO46H2O(Bidepharm Co.,Ltd.,97%),HCl(36%38%,12 molL-1,Greagent)were used as received without furtherpurification.PowderXraydiffraction(PXRD)datawererecorded on a
21、 Rigaku miniflex 600 powder Xray diffractometer(Cu K,=0.154 184 nm)at room temperature(40 kV,15 mA,2=350).The IR spectrum wasrecorded on a Thermo Fisher Nicolet iS 50IR spectrophotometer in a range of 4004 000 cm-1.Thermogravi2210第11期metric analysis(TGA)was carried out on a TGA 50thermogravimetric a
22、nalyzer from 30 to 800 in anargon atmosphere with a heating rate of 5 min-1.The emission spectra and excitation spectra were collected at room temperature using a spectrometer(FLS980,Edinburgh Instruments)equipped with both continuous(450 W)and microsecond pulsed xenon(Xe)lamps,with the detection of
23、 emission spectra to 2 100nm and timecorrelated singlephoton counting lifetimemeasurements as short as 30 ps.Measurements of theemission spectra were conducted using excitation atthe strongest excitation wavelength,i.e.,328 nm for 1and 276 nm for 2.The photoluminescence decay spectra were collected
24、on the same spectrofluorometer withan excitation wavelength of 350 nm as the lightingsource.Quantum efficiency was measured at room temperature with an FLS 980 spectrometer.It is defined asthe ratio between the number of photons emitted by theLn3+ion to the number of those absorbed and could becalcu
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