Ca0.7Sr0.3MoO4：Eu3+红色荧光粉发光性能的改进

采用水热法制备了 Ca0.70Sr0.18MoO4：Eu0.083+, Ca0.70Sr0.18?1.5xMoO4：Eu0.083+, Lax3+与 Ca0.70Sr0.18?yMoO4：Eu0.083+, La0.043+, Nay+红色荧光粉。用 X 射线衍射、扫描电子显微镜、荧光分光光度计对样品的物相、形貌以及发光性能进行测试和表征。结果表明：La3+离子的共掺杂可显著增强 Eu3+离子的发光性能。当 La3+的掺杂量为4％(摩尔分数)时,在395 nm 激发下,位于616 nm处的主发射峰的相对发光强度最大。另外,电荷补偿剂 Na+的引入,也明显增强了荧光粉的发光强度,荧光粉的最高发光强度是未引入 Na+荧光粉的1.47倍。     

La_2(MoO_4)_3:Eu~(3+)纳米红色荧光粉的合成及其发光特性

以水合硝酸镧、水合硝酸铕、硬脂酸和水合钼酸钠为反应物,采用溶剂热法合成了Eu~(3+)离子掺杂的La_2(MoO_4)_3:Eu~(3+)纳米红色荧光粉。利用TEM、XRD、FL对其形貌、结构和发光性能进行了表征。考察了溶剂种类、反应时间、反应温度、Eu~(3+)掺杂量对产物微观形貌和发光性能的影响。结果表明:以异丙醇为溶剂、反应温度180℃、反应时间12 h条件下,得到的样品结晶度高、分散性好、形貌均一,粒径小于100 nm。该样品可被近紫外光(波长391.0 nm)和蓝光(波长462.5 nm)有效激发,最大发射波长位于613.5 nm,为窄带的红光。La_2(MoO_4)_3:Eu~(3+)的发光强度与Eu~(3+)离子掺杂量有关,其最佳掺杂摩尔分数xEu~(3+)=0.15{xEu~(3+)=n(Eu~(3+))/[n(Eu~(3+))+n(La~(3+))]}。     

Ca_(0.7)Sr_(0.3)MoO_4:Eu~(3+)红色荧光粉发光性能的改进（英文）

采用水热法制备了Ca0.70Sr0.18Mo O4:Eu0.083+,Ca0.70Sr0.18-1.5xMoO4:Eu0.083+,Lax3+与Ca0.70Sr0.18-yMo O4:Eu0.083+,La0.043+,Nay+红色荧光粉。用X射线衍射、扫描电子显微镜、荧光分光光度计对样品的物相、形貌以及发光性能进行测试和表征。结果表明:La3+离子的共掺杂可显著增强Eu3+离子的发光性能。当La3+的掺杂量为4%(摩尔分数)时,在395 nm激发下,位于616 nm处的主发射峰的相对发光强度最大。另外,电荷补偿剂Na+的引入,也明显增强了荧光粉的发光强度,荧光粉的最高发光强度是未引入Na+荧光粉的1.47倍。     

LED用的Gd2(MoO4)3:Eu3+红色荧光粉的制备和性能研究

本文利用液相沉积法合成白光LED用的Gd2(MoO4)3:Eu3+红色荧光粉,利用X射线衍射、荧光光谱以及扫描电镜进行系列表征,系统研究掺杂离子浓度、退火温度等条件对Gd2(MoO4)3:Eu3+荧光粉的发光性能影响。结果表明:当pH=7,退火温度为1100℃,Gd:Eu摩尔比例为1.8:0.2时,所合成的荧光粉为正交晶系的类白钨矿结构Gd2(MoO4)3化合物(20-0408),荧光粉在395 nm左右有高的激发效率,发射主峰位置位于615 nm是近紫外LED中一种比较有应用价值的红色荧光粉。     

白光LED用红色发光材料CaLa_2(MoO_4)_4:Eu~(3+)的微波辅助溶胶–凝胶法合成及发光特性

以柠檬酸为络合剂,采用微波辅助溶胶–凝胶法制备了CaLa2(MoO4)4:Eu3+红色荧光粉。研究了前驱体的热分解历程,分析表征了样品的结构、形貌和发光性能。探讨了焙烧温度、Eu3+掺杂量、柠檬酸与乙二醇摩尔比和硼酸用量等对样品发光性能的影响。结果表明:前驱体经700~900℃焙烧均能得到目标产物CaLa2–x(MoO4)4:x Eu3+,样品具有白钨矿结构,属于四方晶系。样品的激发光谱在250~350 nm处有一宽吸收带,对应于Mo–O,Eu–O电荷迁移带;在395和464 nm处存在很强的吸收峰,归属于Eu3+的4f–4f跃迁。发射光谱主峰位于616 nm处,归属于Eu3+的5D0→7F2电偶极跃迁发射。前驱体经800℃焙烧所得样品发光强度最大,且发光强度随着Eu3+掺杂量的增加而增大,在x=0.2~1.0范围内未出现猝灭现象。体系中加入适量乙二醇,可以起到细化晶粒、提高粉体分散性的作用,但浓度过高则会降低样品的发光强度;助熔剂硼酸的用量对样品发光强度影响较大,当用量为3%时,样品的发光性能较好。     

NaGd(MoO4)2∶Eu3+发光粉的水热合成与发光性质

采用水热法,柠檬酸钠为络合剂合成出系列NaGd(MoO4)2∶Eu3+发光粉.利用X射线衍射(XRD)、扫描电镜(SEM)和荧光光谱等对NaGd(MoO4)2∶Eu3+发光粉的结构、形貌和发光性能进行了表征.XRD分析结果表明:所有样品均为单一NaGd(MoO4)2相.SEM结果显示:NaGd(MoO4)2∶Eu3+发光粉的形貌与柠檬酸钠的用量相关.发射光谱和激发光谱的研究结果表明:特征发射峰来自于Eu3+的5D0-7F跃迁.宽的激发带主要来自Eu-O和MoO的电荷迁移带.柠檬酸钠为络合剂合成的样品,发光强度和激发强度下降.讨论了柠檬酸钠对结构、形貌和发光性能的影响.     

溶剂热法制备NaBiF_4:Yb~(3+)/Er~(3+)及掺杂Rb~+离子增强其上转换荧光

采用溶剂热法合成了Na Bi F_4:Yb~(3+)/Er~(3+)上转换发光纳米材料,讨论了在溶剂热阶段反应温度、反应时间对Na Bi F_4:Yb~(3+)/Er~(3+)物相组成、形貌及发光性能的影响。结果表明:在反应阶段,适当增加反应温度、延长反应时间,可以增强Na Bi F_4:Yb~(3+)/Er~(3+)的结晶度,进而提高上转换发光效率,但溶剂热阶段反应温度高于220℃时,容易生成金属铋。此外,通过Rb~+离子掺杂可进一步增强Na Bi F_4:Yb~(3+)/Er~(3+)的上转换发光强度。Rb~+掺杂量为5%(摩尔分数)时,绿光和红光分别增加至原来的1.73和1.5倍。最后基于荧光强度比(I_(FIR))技术,研究了样品在300～500 K温度范围的I_(FIR)变化曲线,结果表明:Na Bi F_4:Yb~(3+)/Er~(3+)样品在温度传感领域有潜在应用价值。     

BaWO4:Eu3+/Tb3+荧光粉的制备及其发光性能的研究

采用共沉淀法制备了Eu3+、Tb3+单掺或双掺的BaWO4荧光粉,探究了Eu3+的掺杂浓度、退火温度及Eu3+和Tb3+掺杂摩尔比对荧光粉发光性能的影响.实验结果表明,当反应温度为500℃、退火时间为2h、Eu3+掺杂浓度为5 mol％时,荧光粉发光强度最强.XRD结果表明,样品为立方晶系的BaWO4相.在掺杂Eu3+...     

LiCaPO4:Eu3+荧光粉的制备及其发光性能的研究

用溶胶凝胶法制备了Eu3+单掺LiCaPO4荧光粉,探究了Eu3+的掺杂浓度、退火温度对荧光粉发光性能的影响.实验结果表明,当反应温度为900℃、退火时间为2 h、Eu3+掺杂浓度为5mol％时,荧光粉发光强度最强.XRD结果表明,样品为六方晶系Ca3(PO4)2与LiCaPO4的混相.利用CIE进行计算,结果表明,E...     

高效红色荧光粉Li1-xAlSiO4+x:xEu3+的制备与发光性能研究

以碳酸锂、氧化铝、二氧化硅、Eu2O3为原料，采用传统高温固相法在较低温度下制备Eu3+离子掺杂LiAlSiO4红色荧光粉，并通过XRD、SEM和光致发光光谱分别对其晶体结构，粉体形貌和发光性能进行表征。结果表明：Eu3+离子掺杂浓度低于15%时，样品为单一基质；样品可以被近紫外350~420nm波段高效激发，最强激发峰位置位于394nm，发射光谱呈现出Eu3+的特征峰，谱带峰值位置在593 nm、616 nm，分别对应于Eu3+的5D0→7F1、5D0→7F2特征跃迁。最强发射对应的掺杂摩尔百分含量为12%，浓度猝灭的发生主要是因为四极-四极（q-q）相互作用，CIE坐标为（0.6464，0.3526），可应用于近紫外芯片激发LED用红色荧光粉。     

Ferroelectric Ceramics in the PbMg1/3Nb2/3O3-PbCd1/3Nb2/3O3 System

Solid solutions (1-x)PbMg_1/3Nb_2/3O₃ + xPbCd_1/3Nb_2/3O₃ with x = 0-0.30 are investigated with purpose to work out a capacitor ceramics with good dielectric properties and low sintering temperature. It is found that the perovskite phase forms at sintering near to 980°C and begins to decompose at higher temperatures. When x grows from 0 to 0.30, the Curie temperature linearly grows from -10°C to +25°C, the dielectric permittivity ε_m in the Curie point T_C decreases from 18000 to 6800 and the phase transition becomes more diffused. The dielectric permittivity at room temperature is rather high and the temperature stability is improved. The system is of interest, because it can serve as a base for working out some ceramic materials for capacitors with low sintering temperature, which needs of no special atmosphere at burning.     

3-溴甲基-3-甲基氧杂环丁烷的合成

以2,2-二溴甲基丙醇（BBMP）为初始原料,通过与碱发生关环反应生成3-溴甲基-3-甲基氧杂环丁烷（BrMMO）。讨论了碱的种类和用量对BBMP关环产率的影响以及反应体系中碱的浓度、反应温度和反应时间对合成BrMMO产率的影响。通过实验确定的最佳工艺条件为：BBMP与NaOH摩尔比为1.0∶1.1,NaOH醇溶液的质量分数为12%,反应温度为78℃,反应时间为4h时,BrMMO产率为65%。最终产品经元素分析、IR和1HNMR检测确定为BrMMO。该试验工艺简单,原料易得,且溶剂便于回收、污染小。     

3-叠氮甲基-3-甲基氧丁环的合成

以三羟甲基乙烷与碳酸二乙酯为原料,经环化反应合成了3-羟甲基-3-甲基氧丁环(HMM O)。在低温下,HMM O与对甲苯磺酰氯反应生成3-磺酸酯甲基-3-甲基氧丁环(M TM O)。M TM O和叠氮化钠发生叠氮化反应形成叠氮单体3-叠氮甲基-3-甲基氧丁环(AMM O)。三步反应收率分别为76%,96%,85%。用核磁、红外、元素分析和DSC表征了化合物的结构与性能。结构鉴定表明为目标化合物AMM O。     

Tunable color emission in LaScO3:Bi3+,Tb3+,Eu3+ phosphor

LaScO₃:xBi³⁺,yTb³⁺,zEu³⁺ (x = 0 − 0.04, y = 0 − 0.05, z = 0 − 0.05) phosphors were prepared via high-temperature solid-state reaction. Phase identification and crystal structures of the LaScO₃:xBi³⁺,yTb³⁺,zEu³⁺ phosphors were investigated by X-ray diffraction (XRD). Crystal structure of phosphors was analyzed by Rietveld refinement and transmission electron microscopy (TEM). The luminescent performance of these trichromatic phosphors is investigated by diffuse reflection spectra and photoluminescence. The phenomenon of energy transfer from Bi³⁺ and Tb³⁺ to Eu³⁺ in LaScO₃:xBi³⁺,yTb³⁺,zEu³⁺ phosphors was investigated. By changing the ratio of x, y, and z, trichromatic can be obtained in the LaScO₃ host, including red, green, and blue emission with peak centered at 613, 544, and 428 nm, respectively. Therefore, two kinds of white light-emitting phosphors were obtained, LaScO₃:0.02Bi³⁺,0.05Tb³⁺,zEu³⁺ and LaScO₃:0.02Bi³⁺,0.03Eu³⁺,yTb³⁺. The energy transfer was characterized by decay times of the LaScO₃:xBi³⁺, yTb³⁺, zEu³⁺ phosphors. Moreover absolute internal QY and CIE chromatic coordinates are shown. The potential optical thermometry application of LaScO₃:Bi³⁺,Eu³⁺ was based on the temperature sensitivity of the fluorescence intensity ratio (FIR). The maximum S_a and S_r are 0.118 K⁻¹ (at 473.15 K) and 0.795% K⁻¹ (at 448.15 K), respectively. Hence, the LaScO₃:Bi³⁺,Eu³⁺ phosphor is a good material for optical temperature sensing.     

2,2,3-三氯-3-苯基-3-(3-甲基苯甲酰基)丙腈的合成研究

以苯甲酰氯、四氯化碳、间甲基苯甲酰氰为原料,合成了标题化合物。重点考察了氰化过程中不同原料配比、反应温度、时间、溶剂和催化剂用量对收率的影响。实验结果表明,其最佳反应条件为:n(1,1,2-三氯-2-苯基乙烯)∶n(3-甲基苯甲酰氰)=1∶1.2,二氯甲烷为反应溶剂,3 mmol催化剂三乙胺,室温反应5 h,总收率达80.6%。     

3-溴甲基-3-甲基氧杂环丁烷的合成

以2,2-二溴甲基丙醇(BBMP)为初始原料,通过与碱发生关环反应生成3-溴甲基-3-甲基氧杂环丁烷(BrMMO).讨论了碱的种类和用量对BBMP关环产率的影响以及反应体系中碱的浓度、反应温度和反应时间对合成BrMMO产率的影响.通过实验确定的最佳工艺条件为:BBMP与NaOH摩尔比为1.0∶1.1,NaOH醇溶液的质量分数为12%,反应温度为78℃,反应时间为4 h时,BrMMO产率为65%.最终产品经元素分析、IR和1HNMR检测确定为BrMMO.该试验工艺简单,原料易得,且溶剂便于回收、污染小.     

Ba3Tb(BO3)3:Eu3+的制备与发光性质

采用高温固相法合成了Ba3Tb(BO3)3:Eu3+红色荧光粉,并研究了Ba3Tb(BO3)3:Eu3+的发光特性。Ba3Tb(BO3)3:Eu3+的激发光谱包含250nm～330nm和350nm～400nm的2个宽带,最大峰值位于383nm,可以被紫外-近紫外发光二极管(light-emitting diodes,LED)有效激发。Ba3Tb(BO3)3:Eu3+的发射谱显示出4组发射峰,其主发射峰位于620nm,对应Eu3+的5D0→7F2跃迁;Eu3+掺杂摩尔分数为2%时,Ba3Tb(BO3)3:Eu3+发光亮度最高。经分析发现Ba3Tb(BO3)3:Eu3+存在Tb3+→Eu3+的能量传递。     

The Preparation and Crystal Structure of TlMnCl3, TlFeCl3, TlCoCl3 and TlNiCl3

The compounds TlMnCl₃, TlFeCl₃, TlCoCl₃ and TlNiCl₃ were prepared by heating T1C1 with the corresponding transition metal dichloride in an evacuated ampoule. Atomic positions were determined from powder photographs. All four compounds were found to be related to the perovskite type structure. TlMnCl₃ has a cubic structure, space group Pm3m, with a_o = 5.025 Å. The other three compounds are hexagonal, probable space group P6₃mc, with cell dimensions (in Å) a₀ = 6.976 and c₀ = 6.008 for the Fe compound, a₀ = 6.907 and c₀ = 5.981 for the Co compound and a₀ = 6.863 and c₀ = 5.881 for the Ni compound. The three hexagonal compounds are isomorphous. A measureable concentration of basal plane stacking faults was found to occur in TlFeCl₃ and also, to a lesser degree, in TlCoCl_3.     

Thermal analyses of poly(3-hydroxybutyrate), poly(3-hydroxybutyrate-co-3-hydroxyvalerate), and poly(3-hydroxybutyrate-co-3-hydroxyhexanoate)

Thermal analyses of poly(3-hydroxybutyrate) (PHB), poly(3-hydroxybutyrate-co-3-hydroxyvalerate) [P(HB–HV)], and poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) [P(HB–HHx)] were made with thermogravimetry and differential scanning calorimetry (DSC). In the thermal degradation of PHB, the onset of weight loss occurred at the temperature (°C) given by T_o = 0.75B + 311, where B represents the heating rate (°C/min). The temperature at which the weight-loss rate was at a maximum was T_p = 0.91B + 320, and the temperature at which degradation was completed was T_f = 1.00B + 325. In the thermal degradation of P(HB–HV) (70:30), T_o = 0.96B + 308, T_p = 0.99B + 320, and T_f = 1.09B + 325. In the thermal degradation of P(HB–HHx) (85:15), T_o = 1.11B + 305, T_p = 1.10B + 319, and T_f = 1.16B + 325. The derivative thermogravimetry curves of PHB, P(HB–HV), and P(HB–HHx) confirmed only one weight-loss step change. The incorporation of 30 mol % 3-hydroxyvalerate (HV) and 15 mol % 3-hydroxyhexanoate (HHx) components into the polyester increased the various thermal temperatures T_o, T_p, and T_f relative to those of PHB by 3–12°C (measured at B = 40°C/min). DSC measurements showed that the incorporation of HV and HHx decreased the melting temperature relative to that of PHB by 70°C. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 82: 90–98, 2001