新型红色荧光粉NaLa(MoO4)2∶Sm3+的微波辅助溶胶-凝胶法合成及发光性能研究

采用微波辅助溶胶-凝胶法合成了NaLa(MoO4)2∶Sm3+新型系列红色荧光粉.通过热重-差热分析仪分析了前驱体的热分解过程,运用X射线衍射仪、扫描电镜及荧光分光光度计等手段分别对样品的物相结构、微观形貌、发光性质等进行分析表征.结果表明:前驱体在700℃以上煅烧即可得到NaLa(MoO4)2的纯相;800℃煅烧所得样品粒度均匀,尺寸约为700～ 800 nm;所合成的NaLa(MoO4)2∶Sm3+主要的激发峰位于307 nm、364 nm、377 nm、405 nm、469 nm处,其中最强的激发峰位于405 nm;发射光谱主要由571 nm、607 nm、647 nm处的三个发射峰组成,分别对应Sm3+的4G5/2→6H5/2、4G5/2→6H7/2、4G5/2→6H9/2跃迁,其中最强发射峰位于647 nm处,说明样品在紫外、近紫外及蓝光区均可被激发,且发出红光.研究发现:煅烧温度为800℃、Sm3+掺杂浓度为0.04时,样品发光强度最大,其浓度淬灭主要是由电偶极-电偶极相互作用引起的.     

橙红色荧光粉Ca10Li(PO4)7∶Sm3+的合成及其发光特性研究

采用固相法合成了Ca10Li(PO4)7∶xSm3+橙红色荧光粉,研究了材料的发光性质.结果表明,以404 nm近紫外光作为激发源时,Ca10Li(PO4)7∶xSm3+表现为多峰特征,主峰位于569 nm、606 nm、651 nm和713 nm,分别对应Sm3+的4G5/2→6H5/2、4G5/2→6H7/2,4 G5/2 →6H9/2 and 4 G5/2 →6H11/2跃迁发射,且606 nm发射峰最强,材料发射橙红光;监测606 nm发射峰,对应的激发光谱包含363 nm、376 nm、404 nm和478nm多个激发峰;改变Sm3+的掺杂量,发现Ca10 Li(PO4)7∶Sm3+的发射强度表现出先增大、后减小的变化趋势,x=0.05时发射强度最大,即存在浓度猝灭现象,造成浓度猝灭的机理为电多极相互作用,Ca10Li(PO4)7∶Sm3+的色坐标基本不变,位于橙红色区域.Ca10Li(PO4)7∶Sm3+具有较好的温度特性,激活能为0.188 eV.     

Sm3+掺杂Na0.5Bi0.5TiO3无铅压电陶瓷的发光性能及热稳定性研究

采用传统的固相烧结法,制备了一系列的Sm3掺杂Na0.5Bi0.5TiO3无铅压电陶瓷(NBT∶ xSm3,0.005≤x≤0.04).利用X射线衍射仪和荧光分光光度计分别对NBT∶ xSm3+陶瓷样品的物相结构和光致发光性能以及热稳定性进行了分析.结果 表明,所有样品均为纯的三方钙钛矿结构.样品的激发光谱在480 nm有很强的激发峰,与蓝光LED芯片匹配.发射光谱包含位于563 nm、597 nm、645 nm、709 nm处的四个发射峰,分别归属于Sm3+的4G5/2→6HJ/2(J=5、7、9、11)跃迁,其中发射主峰位于597 nm,呈现橙红色发光.当Sm3+含量为0.02 mol时发光性能最佳.当温度范围在30 ～210℃之间时,NBT∶0.02Sm3陶瓷样品的发光性能具有良好的热稳定性     

LED用红色荧光粉NaGdTiO4∶Sm3+的合成与发光性能

采用高温固相法制备了白光LED用NaGd(1-x)TiO4∶xSm3+系列红色荧光粉,并对样品分别进行了X射线衍射分析和荧光光谱测试.结果表明,样品可以被紫外、近紫外和蓝光有效激发,在409 nm激发下,该荧光粉有三个主要发射峰,位于567 nm、607 nm和652 nm处,分别对应于Sm3+的4G/2→6H5/2、4G5/2→6H7/2、4G5/2→6H9/2的跃迁发射,其中607 nm处发射最强,呈现红色发光.当Sm3+的掺杂浓度为2.5mol;时,达到最佳的发光效果.因此,这种荧光粉是一种有应用潜力的白光LED红色荧光粉.     

近紫外激发的Na2ZnSiO4∶Sm3+橙红色荧光粉的合成及发光性能

采用溶胶-凝胶法制备了适合于近紫外激发的橙红色荧光粉Na2 ZnSiO4∶Sm3+,利用X射线衍射、扫描电镜、荧光光谱对样品的相结构、形貌及发光性能进行了表征.结果表明:制得的样品属于单斜晶系,粒径约为2 μm.样品的激发光谱在330 ～ 550 nm间呈多峰分布.在404 nm近紫外光激发下,发射光谱由峰值为566 nm,604 nm和650 nm的3个峰构成,发射主峰位于604 nm处,对应Sm3+的4 G5/2→6H7/2跃迁,呈橙红光发射.当Sm3+的掺量为3;时,其发光强度达到最大,随后减小,是由电偶极-电偶极相互作用引起的浓度猝灭.     

白光LED用K2Ba(WO4)2∶Sm3+红色荧光粉的制备与表征

采用高温固相法合成了一种新型K2Ba(WO4)2∶xSm3+红色荧光粉.通过XRD、SEM和荧光分光光度计对样品的结构、形貌和发光性能进行了研究.结果表明:该荧光粉具有三方晶系结构,在402 nm处有较强的激发峰,与近紫外LED芯片相匹配.在402 nm激发下,出现了Sm3的4G5/2→6 HJ(J=5/2,7/2,9/2,11/2)的特征跃迁,最强峰位于602 nm处,对应于Sm3+的4G5/2→6H3/2跃迁.Sm3+的最佳掺杂量为x=0.02,且Sm3+之间的临界距离为2.776 nm,浓度猝灭的机理为电偶极-电偶极相互作用.     

Na2SrP2O7∶Sm3+橙色荧光粉的制备与发光性能的研究

利用稀土离子Sm3+作为激活剂,采用传统的高温固相法制备了Na2SrP2O7∶xSm3+(x=0.02mol;)橙色荧光粉.用扫描电镜、X射线衍射仪和荧光分光光度计对粉体的表面形貌、晶体结构和荧光光谱进行了表征.XRD分析和荧光光谱分析得出:最佳的烧结温度为700℃.该荧光粉能够被404 nm光高效激发,发射光谱在可见光区呈三峰发射,峰值位于564 nm、603 nm、647 nm,其最强发射峰位于603 nm处,对应于Sm3的4G5/2→6H7/2特征发射.设定发射波长为603 nm,得到荧光粉的激发光谱为一个主峰位于404 nm的宽带激发峰,表明该荧光粉可被紫外光和近紫外光有效地激发.研究了Sm3+掺杂浓度和助熔剂NH4Cl含量对Na2SrP2O7∶Sm3+橙色荧光粉荧光性能的影响,得出Sm3+的最佳掺杂量为2mol;.3wt;的助熔剂NH4Cl有利于荧光粉颗粒的分散,减小平均粒径,改善晶粒形貌,提高荧光粉的相对发光强度,还能降低制备所需的温度.     

溶胶-凝胶法制备Li2ZnSiO4∶Sm3+红色荧光粉

采用溶胶-凝胶法合成Li2ZnSiO4∶Sm3+红色荧光粉,并对其发光性质进行了研究.结果表明:所得样品为正方晶系,呈柱状颗粒.用566 nm、604 nm和651 nm作为监控波长,激发峰位置和形状并未发生改变,但峰的强度有所差别.激发主峰位于408 nm(6H5/2→4 L13/2)处.在408 nm激发下,样品的发射光谱由四个荧光发射峰构成,分别位于566 nm、604 nm、651 nm和710 nm,对应于Sm3+特征跃迁4 G5/2→6HJ(J=5/2,7/2,9/2,11/2),发射主峰为604nm,是一种适用于白光LED的红色荧光粉,当Sm3+的掺杂浓度为2.5;,发光强度最大.     

花状NaLa(MoO4)2∶Eu3+,M(M=Gd3+,Ti4+)红色荧光粉的水热合成及发光性能

以乙二醇和水的混合溶液为溶剂,采用水热法合成了花状的NaLa(MoO4)2∶Eu3+红色荧光粉.通过X射线衍射仪、扫描电子显微镜、荧光分光光度计等手段对产物进行了分析和表征.结果表明:产物NaLa(MoO4)2∶Eu3+属于四方晶系白钨矿结构.样品分散性好,粒度均匀,呈花状结构.样品的激发光谱分为两部分:位于250～350 nm的宽激发带归属于Eu-O,Mo-O之间的电荷迁移;350～500 nm的系列尖锐峰归属于Eu3+的f-f跃迁.样品的发射光谱中主发射峰位于615 nm处,归属于Eu3的5 Do→7R电偶极跃迁.此外,共掺杂适量的Gd3+或Ti4能够有效敏化Eu3+的发光,明显增强了615 nm的红光发射.     

球形NaY(MoO4)2∶Sm3+荧光粉的合成及荧光性能研究

以水热法合成了球形NaY(MoO4)2∶Sm3+红色荧光粉,通过X-射线衍射(XRD)、场发射扫描电镜(FESEM)、光致荧光光谱(PL)进行表征,考察荧光粉的晶相、形貌及发光性能.研究了Sm3+掺杂浓度对发光性能的影响,通过调节体系酸度对样品形貌进行控制.实验结果表明:180℃水热反应20 h,pH=7.0时控制合成出规则球形NaY(MoO4)2粉体,当Sm3+的摩尔掺杂量为4;时,发射峰强度达到最大,继续增加Sm3+浓度,其发射峰强度减弱,出现了浓度猝灭效应.     

Crystal and Molecular Structure of mer-Co(4-CH3C5H4N)3(N3)3

The crystal structure of mer-Co(4-CH₃C₅H₄N)₃(N₃)₃has been determined by single crystal X-ray methods at 300 K. The compound crystallizes in the monoclinic space group C 2/c, a = 19.087(6), b = 16.769(4), c = 15.845(4) Å, β = 119.04(2)°, V = 4434(2) ų, M_r = 464.42. Z = 8, D_x = 1.391 Mgm⁻³, F(000) = 1920, λ (MoKα) = 0.71069 Å, μ = 0.802 mm⁻¹. The cobalt(III) ions are octahedrally coordinated to three azide groups and to three 4-methyl-pyridine molecules to form isolated coordination polyhedra.     

Crystal Structures of 6-methyl-3-phenylsulfonylchroman-4-one andtrans-6-methyl-3-phenylsulfonylchroman-4-ol

The crystal structures of (i) CH₃(C₉H₆O₂)SO₂C₆H₅ and (ii) CH₃(C₈H₈O₂)SO₂?C₆H₅ have been determined by X-ray diffraction. (i) crystallizes in the monoclinic space groupP2₁/c with unit cell parametersa=8.814(1)Å,b=10.310(1)Å,c=15.841(4)Å, β=98.17(1)^o, andZ=4, and (ii) crystallizes in the orthorhombic space groupP2₁2₁2₁ with unit cell parametersa=6.206(1)Å,b=11.752(5)Å,c=19.865(3)Å, andZ=4. The pyran ring in both of them is in the distorted half-chair conformation with differeing degrees of distortion from the ideal.     

Crystal Structure of Zinc(II) Complexes with 2-Ethyl-3-hydroxy-4H-pyran-4-thione and 2-Ethyl-3-hydroxy-4H-pyran-4-selenone

Crystallography Reports - Zn(II) complexes with 2-ethyl-3-hydroxy-4H-pyran-4-thione, [Zn(ehpt)2], and 2-ethyl-3-hydroxy-4H-pyran-4-selenone, [Zn(ehps)2], were synthesized and characterized by...     

水热法生长非线性光学晶体K4Gd2(CO3)3F4

采用水热法,探索了 K4Gd2(CO3)3F4晶体的析晶条件,诸如生长原料及配比、生长温度、生长周期等,并成功生长了毫米级的透明单晶.对生长的晶体进行了XRD、UV-Vis-NIR、SHG等测试,结果表明,K4Gd2( CO3)3F4晶体在380～2000 nm波段的透过率超过80;,紫外吸收截止边低于200nm;其二阶非线性光学效应约为KDP的3.5倍.     

Dielectric Behaviour of the Nematic Phase of 4-n-Pentyloxyphenyl 4-(3-Bromo-4-n-nonyloxybenzoyloxy)-3-ethyl-benzoate (PBNEB)

Due to the high viscosity of 4-n-pentyloxyphenyl 4-(3-bromo-4-n-nonyloxybenzoyloxy)-3-ethyl-benzoate (PBNEB) the dielectric reorientation processes take place in the kHz and MHz range respectively. We observed two different relaxation ranges in the nematic phase from 10 Hz to 10 MHz if the measuring field is parallel to the director and one relaxation range for the perpendicular orientation. Dielectric measurements at 6.7 GHz demonstrate that at this frequency ϵ′∥ and ϵ′⊥ can be regarded as high-frequency limit. The experimental values are discussed from the point of view of the Meier-Maier theory.     

Crystal Structure and Computational Study of 5-Ethyl-4-(4-Methoxyphenethyl)-4,5-Dihydro-3H-1,2,4-Triazol-3-One and 4-(4-Methoxyphenethyl)-5-Propyl-4,5-Dihydro-3H-1,2,4-Triazol-3-One

Crystallography Reports - Molecular structures of compounds 5-ethyl-4-(4-methoxyphenethyl)-4,5-dihydro-3H-1,2,4-triazol-3-one, (C13H17N3O2) (I) and...     

3-Methyl-3a,4-Dihydro-3H-Thiochromeno[4,3-c]isoxazol

Abstract  The crystal structure of the title compound, C₁₁H₁₁NOS, was determined by an X-ray diffraction analysis. The compound crystallizes in the monoclinic space group P2₁/c with cell parameters a = 10.533(2) ?, b = 12.7826(19) ?, c = 7.6491(17) ?, β = 107.997(17)^°, V = 979.5(3) ?³ and Z = 4. The S containing heterocycle adopts a sofa conformation, whereas the 5-membered ring adopts an envelope conformation. The crystal packing is characterized by weak C–H···N contacts and π-stacking interactions. Graphical Abstract  The title compound, 3-methyl-3a,4-dihydro-3H-thiochromeno[4,3-c]isoxazol was synthesized by an 1,3 dipolar cycloaddition reaction and its crystal structure determined. Single crystal X-ray diffraction analysis reveals that the aromatic 6-membered ring is planar, whereas the ring containing the S atom adopts a sofa conformation and the 5-membered ring an envelope conformation. The methyl group is in an equatorial position.      

Crystal Structure of 3-(4-Methoxy-benzylidene)-isothiochroman-4-one

Abstract  

The title compound, 3-(4-methoxy-benzylidene)-isothiochroman-4-one (C₁₇H₁₄O₂S) was prepared from the reaction of isothiochroman-4-one with benzaldehyde in the presence of small amount of HCl. The structure of the synthesised compound was determined by IR, ¹H NMR and X-ray crystallography. The structure was solved in monoclinic, space group P2₁/n with a = 3.9773 (7) Å, b = 10.918 (2) Å, c = 30.609 (6) Å, β = 90.615 (3)°, V = 1329.1 (4) Å³, Z = 4 and with R _int = 0.047. The bicyclic ring of isothiochroman-4-one moiety does not adopt a planar geometry. The molecular conformation is stable via C10–H···O1 and C16–H···S1 intramolecular hydrogen-bonding interactions. These contacts involve molecules in an extended two-dimensional sheet to the bc plane.     

Mesomorphic Properties of the 4-(4-n-Alkoxybenzoyloxy)-Benzylidene-4-n-Alkoxyanilines and 4-(4-n-Alkoxybenzoyloxy)-3-Methoxy-Benzylidene-4-n-Alkoxyanilines

Transition temperatures, transition enthalpies and X-ray results are reported for 4-(4-n-heptyloxybenzoyloxy)-benzylidene-4-n-alkoxyanilines, 4-(4-n-nonoxybenzoyloxy)-benzylidene-4-n-alkoxyanilines and their 3-methoxy-benzylidene substituted derivatives.     

The Electronic Structures of (PH4)3C60 and (ClO4)3C60

Abstract

We have studied theoretically the electronic structures of a hypothetical donor-type material, (PH₄)₃C₆₀, and a hypothetical acceptor-type material, (ClO₄)₃C₆₀ from first principles by using a full-potential linear-combination-of-atomic-orbitals method based on the density-functional theory within the local-density approximation. It is found that the charge transfer from the PH₄ molecules to the C₆₀ molecules is perfect while the charge transfer from the ClO₄ molecules to the C₆₀ molecules is not perfect. We compare the latter result with the electronic structures of two typical acceptor-type organic conductors, (TMTSF)₂ClO₄ and (TMTSF)₂PF₆, and discuss the differences.