Si衬底Al_2O_3:Eu~(3+)薄膜的溶胶-凝胶法制备及其发光性能

采用溶胶-凝胶法在Si衬底上制备Al2O3:Eu3+薄膜;并采用DTA-TG、XRD、SEM、AFM及光致发光光谱对其进行一系列表征,分析Al2O3:Eu3+薄膜的发光机制,探讨热处理温度和Eu3+掺杂浓度对发光性能的影响规律。结果表明,采用溶胶-凝胶法制备工艺,得到发光强度高的Al2O3:Eu3+薄膜,薄膜的最佳激发波长为265nm,Eu3+的最佳掺杂浓度为10mol%,在265nm光激发下,最强的发射峰出现在617nm附近;采用溶胶-凝胶法制备得到Al2O3:Eu3+薄膜表面致密、平整且无裂纹产生,表面粗糙度约为1.4nm,有利于硅基光电子器件的制备和应用。     

Photoelectric properties of thin Eu3+-doped TiO2 films sensitized by cis-RuL2(SCN)2·2H2O

Thin nanocrystalline TiO2 films doped by europium ions (Eu3+) were obtained by the sol-gel method. The photoelectric properties of Eu3+-doped TiO2 film electrode sensitized by cis-RuL2(SCN)2·2H2O(L=cis-2,2'-bipyridine-4,4'-dicarboxlic acid) ruthenium complex were studied. The thin filmswere characterized by X-ray diffraction, atomic force microscopy and X-ray photoelectron spectroscopy. Effect of doping Eu3+ on microscopic structure and photoelectrical properties were discussed. The result shows that doping europium ions makes specific surface area of these films larger, which contributes toimproving the photoelectric properties. It is found that an optimal compositiondoped with 0.2 mol.% Eu3+ exhibits the highest photoelectric properties. I sc is 0.37 mA·cm-2 , which is 0.17mA·cm-2 bigger than that of un-doped films;Voc is 405 mV, which is 50 mV bigger than thatof un-doped films.     

Crystal Structures of Dy_2(WO_4)_3 and GdY(WO_4)_3

Two compounds, Dy2(WO4)3 and GdY(WO4)3, were synthesized by using the standard solid state reaction technique. The crystal structure was determined by powder X-ray diffraction and Rietveld refinement method. It is found that both compounds have Eu2(WO4)3-type monoclinic structure, with space group C 2/c, Z = 4. The unit cell parameters of Dy2(WO4)3 are a = 0.75981(1) nm. b = 1.13220( 1) nm, c = 1.13254( 1) nm, and β= 109.8001(3)°, and those of GdY(WO4)3 are a = 0.76175(1) nm, b = 1.13543(1) nm, c = 1.13496(2) nm, and bbbbbbbbbβwhile each rare-earth atom is surrounded by eight oxygen atoms. WO4 tetrahedra share their four vertices with REO8 (RE = Dy, Gd, or Y) trigondodecahedra and some REO8 trigondodecahedra share an edge with each other. The phase transition and the magnetic properties were investigated by differential thermal analysis (DTA) and dc superconducting quantum interference device (SQUID) magnetometer.     

掺杂的SrAl2O4:Eux2+,Dyy3+长余辉粉的合成、表征及发光性质

采用自蔓延高温合成法制备了组成为SrAl2O4:Eu2+x,Dy3+y的2组(x:y=1:1,x:y=1:2)12种铝酸锶长余辉发光粉,测试结果表明,组成为SrAl2O4:Eu2+0.0125,Dy3+0.0125的发光亮度最好。以上述配比为依据,又分别引入了可以用于制备荧光材料的阳离子Li+、Be2+,以及既可以用于制备荧光材料也可以用于制备自激活荧光材料的阳离子Zn2+、Cd2+、Pb2+,共制得5个系列22种铝酸锶(SrAl2O4)长余辉发光粉。Zn2+0.0125的掺杂使得SrAl2O4:Eu2+0.0125,Dy3+0.0125的余辉亮度得到大幅度提高,而且SrAl2O4:Eu2+0.0125,Dy3+0.0125,Zn2+0.0125的衰减速度也明显慢于SrAl2O4:Eu2+0.0125,Dy3+0.0125。X射线衍射结果表明,掺杂少量稀土离子(Eu2+和Dy3+)不会改变SrAl2O4基质的晶体结构。另外,透射电镜分析和粒度分布结果表明,产物为疏松多孔的蘑菇云状固体,粒度在10μm左右。     

Ag+掺杂ZnWO4纳米棒的微波水热法合成及光催化性能

以硝酸锌(Zn(NO3)2·6H2O)、和钨酸钠(Na2WO4·2H2O)作为起始反应物,利用微波水热法在200℃下合成纳米棒状钨酸锌。利用X-射线粉末衍射、场发射扫描电子显微镜、透射电子显微镜及能谱成分图谱等分析手段对纳米棒状钨酸锌粉体进行表征,并对不同Ag+掺杂量的ZnWO4纳米棒的光催化性能进行了研究。结果表明:Ag+成功的掺入ZnWO4纳米棒中;随着Ag+掺杂量的增加ZnWO4纳米棒的颗粒尺寸也不断增大;Ag+掺杂量2%时纳米棒状钨酸锌粉体的光催化性能最优,但是随着掺杂量的逐渐增加光催化性能反而降低。     

白光LED用新型红色荧光粉SrMgSi2O6:Eu3+, M(M=Gd3+, Ti4+)的合成及性质

以Na2CO3为电荷补偿剂,采用凝胶-燃烧法合成新型红色硅酸盐发光材料SrMgSi2O6:Eu3+。用X射线粉末衍射仪、荧光分光光度计等对合成产物进行分析和表征。结果表明：SrMgSi2O6:Eu3+ 的晶体结构与Sr2MgSi2O7相同,同属四方晶系。样品SrMgSi2O6:Eu3+的激发光谱在220～300 nm出现一宽带吸收,归属于O2--Eu3+之间的电荷迁移,300 nm以后出现的锐线峰为Eu3+的f-f跃迁吸收峰,其最强锐线峰位于400 nm,因而,可以被InGaN管芯产生的紫外辐射有效激发。发射光谱由两个强发射峰组成,位于592和618 nm处,分别属于典型的Eu3+的5D0→7F1和5D0→7F2跃迁。此外,研究发现：共掺Gd3+或Ti4+均能敏化Eu3+的发光,可有效提高样品的红光发射。因此,SrMgSi2O6:Eu3+, M(M=Gd3+, Ti4+)有望成为一种与InGaN管芯匹配的白光LED用红色荧光粉     

LaMgAl11O19: Mn2+和LaMgAl11O19:RE, Mn2+(RE=Eu2+, Gd3+)的发光特性

以H3BO3作助熔剂,用高温固相法在1150℃、保温4 h的条件下成功制备了LaMgAl11O19:Mn的单相粉末样品并研究了其真空紫外光激发下的一系列发光特性.在紫外光(254 nm)激发下,LaMgAl11O19:Mn不发光;真空紫外光(147 nm)激发下,观察到Mn2+很强的3d5→3d44s的跃迁发光,峰值位于516 nm,结果表明,Mn2+的掺杂浓度在0.05 mol/mol时发光最强.为了继续增强LaMgAl11O19中Mn2+的发光强度,在固定Mn2+的浓度为0.05 mol/mol的条件下又合成了LaMgAl11019:(Eu2+,Mn2+)与LaMgAl11O19:(Gd3+,Mn2+),利用(Eu2+,Mn2+)和(Gd3+,Mn2+)间存在有效的能量传递的特性,很好的达到了增强Mn2+的发光的目的.     

Hydrothermal synthesis and characterization of Eu-doped GaOOH/α-Ga2O3/β-Ga2O3 nanoparticles

Eu-doped GaOOH nanoparticles with size of 5-8 nm were prepared by hydrothermal method using sodium dodecylbenzene sulfonate (SDBS) as surfactant. Eu-doped α-Ga₂O₃ and β-Ga₂O₃ were further fabricated by annealing GaOOH:Eu and then characterized by X-ray diffraction(XRD), transmission electron microscopy (TEM) and photoluminescence (PL). The TEM results show that monodisperse Eu³⁺-doped GaOOH nanoparticles form and then transform into Eu³⁺-doped α-Ga₂O₃ and β-Ga₂O₃ through annealing the GaOOH:Eu nanoparticles at 600 and 900 °C, respectively. PL studies indicate that GaOOH:Eu has the highest intensity at 618 nm. Luminescence quenching is observed at higher Eu³⁺ concentration in all samples.     

氧化钨/碳SPS原位合成WC硬质合金的XPS研究

以WO3＋14.5%C（质量分数,下同）的混合粉作为原始粉末,采用放电等离子烧结（SPS）在不同温度下烧结保温3 min,直接一步合成致密WC硬质合金.借助于X射线光电子能谱（XPS）分析了合成样品的元素价态变化,探讨了SPS原位合成的过程和机理.结果表明：随着烧结温度的升高,样品中的W元素的价态逐步由氧化态的W＋6,W^＋5,W^＋4过渡到单质W^0＋和碳化物态的W^＋2;而样品中的碳元素价态却逐步由单质碳转变为化合碳,氧化物态的晶格氧强度逐渐降低,以碳氧键存在吸附的氧强度逐渐增强.XPS分析结果表明,在SPS原位合成中,WO3首先被碳还原,并经历了一系列中间钨氧化物状态后得到金属钨,然后金属钨进一步发生碳化反应最终形成WC.     

Ba2+替代对Sr4Al14O25:Eu2+, Dy3+结构和发光性能的影响

采用高温固相反应按化学式Sr4-xBaxAl14O25: Eu2+, Dy3+(x＝0, 0.8, 1.6, 2.4, 3.2, 4) 配比原料,合成长余辉发光材料。X射线衍射分析表明,当x＝0.8时,产物物相为单斜结构SrAl2O4和磁铅矿结构SrAl12O19共存;当x>1.6时,产物主相转变为BaAl2O4六角结构。对所得样品采用360 nm光照,发射光谱表明,样品发光是以Eu2+为发光中心,由Eu2+电子4f65d-4f7跃迁所致,并且随着Ba掺入量的增加,样品发射光谱峰位产生移动,这是由于Sr2+取代产物中Ba2+位置后,导致晶格收缩,影响Eu2+的5d能级劈裂,从而影响电子4f65d-4f7跃迁。余辉光谱显示x>1.6时,产物的余辉发光是以BaAl2O4基质中Eu2+为发光中心。余辉衰减检测和热释光谱分析发现不同掺Ba量的样品余辉衰减快慢不同,是由于其中存在的陷阱能级深度不同,且陷阱能级越深,其余辉时间越长     

硬质合金用纳米级（W,Ni,Fe,V）系复合氧化物粉末的制备

用Ｈ２ＷＯ４,ＮｉＣｌ２,可溶性盐的碱性水溶液与ＦｅＣｌ２水溶液快速混合的方法,在超声喷雾热转换装置中制备（Ｗ,Ｎｉ,Ｆｅ,Ｖ）系纳米级复合氧化物粉末。通过Ｘ射线衍射及透射电镜分析,研究了复合粉末的物相组成、颗粒形貌及粒径范围。结果表明,采用上述两种溶液快速混合及超声喷雾热转换的方法,可以制备出成分均匀的复合氧化物粉末,其物相组成为ＷＯ２．９２,ＮｉＯ,Ｖ２Ｏ３,粉末的千粒平均粒径为３２ｎｍ,颗粒     

Preparation and luminescent properties of Eu doped Sr3La(PO4)3 phosphor

Eu²⁺-doped Sr₃La(PO₄)₃ phosphors were synthesized by solid-state reaction method. Their luminescent properties were investigated. The phosphor could be excited by ultraviolet light effectively. The emission spectra exhibit two emission peaks located at 418 nm and 500 nm, respectively. These two peaks originated from two different luminescent centers, respectively. One is nine-coordinated Eu(I) center, other is six-coordinated Eu(II) center. It was found that the doping concentration of Eu²⁺ ions affected the shape of emission spectra. As the doping concentration increasing, Eu²⁺ ions are more likely to form Eu(I) luminescent centers and emit purple light.     

化学共沉淀法制备BaAl_2Si_2O_8:Eu~(2+)荧光粉及其发光特性

采用化学共沉淀法一次煅烧工艺制备BaAl2Si2O8:Eu2+荧光粉。用X射线衍射仪、荧光分光光度计和扫描电镜等对BaAl2Si2O8:Eu2+荧光粉的相结构、发光性能、形貌进行表征。结果表明,化学共沉淀法合成了单相的BaAl2Si2O8:Eu2+,且粒度小,分布均匀,呈类球形。在320nm激发下,其发射主峰位于465nm附近,当Eu2+的掺杂浓度为3.5%,发光强度达到最大值,猝灭浓度有所提高,这主要是由于纳米微粒边界对能量共振传递的阻断和猝灭中心在纳米晶内分布的涨落性引起的。     

溶胶-凝胶法制备Pt2+掺杂Bi2O3及光催化性能研究

用溶胶-凝胶法制备了Pt2+掺杂的Bi2O3光催化剂(Pt/Bi原子比分别为1/100、2/100、3/100和4/100),以甲基橙为模拟有机污染对催化剂的光催化性能进行了考察。光催化剂用BET、XRD、XPS和紫外-可见漫反射进行了表征,结果表明Pt/Bi原子比为3/100时催化剂的比表面最高;经500℃焙烧后光催化剂晶型为α-Bi2O3;掺杂Pt2+后Bi2O3在可见光区的吸收增强;掺杂Pt2+后Bi 4f7/2和O 1s结合能均向低能端偏移,催化性能测试结果表明Pt/Bi原子比为3/100时的催化剂活性最高。增加的比表面、对可见光响应增强和结合能向低能端偏移均有利于提高Bi2O3光催化活性。     

Na2O-CaO-SiO2系透明微晶玻璃制备及其微观结构

制备了Yb3+掺杂的Na2O-CaO-SiO2系高结晶度、透明微晶玻璃。用差热分析(DSC)初步确定基础玻璃的核化及晶化温度范围,用X射线衍射(XRD)测定微晶玻璃析出晶相,用扫描电镜(SEM)研究微晶玻璃的微观结构。结果表明:组成为53SiO2-30CaO-17Na2O(摩尔分数,%)的基础玻璃经热处理析出了Na4Ca4Si6O18晶相;合适热处理制度为:595℃核化5 h,730℃晶化1 h;所制备的微晶玻璃析晶度高,晶粒尺寸约100μm,微晶玻璃仍具有较高的透明度。     

Degradation of BPB in photocatalysis enhanced by photosensitizer

The treatment of wastewater containing bromphenol blue （BPB） by WO3/α-Fe203 was studied. Reaction mechanism of photocatalysis enhanced by photosensitizer was probed. The relationships between the composition of heterogeneous photocatalyst, the starting concentration of BPB, amount of photocatalyst, pH, amount of H2O2, illumination time and the decoloring rate of BPB were discussed. The results show that the decoloring rate of BPB can reach 99.1% by using WO3/α-FeaO3 as heterogeneous photocatalyst, with the composition of m（WO3）：m（α-Fe2O3 ）=3：1, the initial concentration of BPB = 15mg/L, the amount of catalyst = 0.300 g, pH= 6.3, the amount of H2O2 =0.2 mL, and the illumination time = 6 h.     

碳含量对盐助燃烧合成法制备的超细WC粉体形貌、尺寸和相的影响

在WO3-Mg-C-Na2CO3体系中,引入NaCl做稀释剂,通过盐助燃烧合成法制备了超细碳化钨（WC）粉体。利用扫描电镜（SEM）、能谱仪（EDS）和X射线衍射（XRD）对产物进行分析,研究了碳（C）含量对制备的WC粉体的形貌、尺寸和相的影响。结果表明：在m=0.125（Na2CO3的摩尔数）基础上,将原料中碳的摩尔数从l=2增加到2.25和2.5,浸出前产物由少量大尺寸颗粒及大量小尺寸颗粒组成;浸出后产物是由亚微米小颗粒团聚而成,颗粒之间熔化烧结现象很弱,呈弱团聚状态;浸出产物的粒度分布基本符合正态分布,尺寸在200～350nm的范围内;在l=2.25条件下,合成的产物主要为目标产物WC,副产物W2C含量极少。即k=2.0（NaCl的摩尔数）,m=0.125,l=2.25为制备单相WC的工艺条件。     

掺钽钨青铜(Ta_xWO_3)的水热合成及电催化性能

以TaCl5和Na2WO4×2H2O为原料,采用水热法在170℃制备性能良好的掺钽钨青铜。并利用XRD、TEM、SEM、UV-vis、IR等谱等分析检测手段对样品的结构和形貌等进行表征,同时研究了掺钽钨青铜的电催化还原氢的性能。结果表明:在170℃合成六方相的掺钽钨青铜,尺寸为10~50 nm。电催化还原氢的实验显示,掺钽钨青铜对氢具有很强的电催化还原活性。     

Photocatalytic degradation of MO by complex nanometer particles WO3/TiO2

Complex nanometer particles WO3/TiO2 were prepared using a sol-gel process and characterized using XRD spectra. The photocatalytic activity of TiO2 can be increased by doping W^6＋ with TiO2 because the doped W^6＋ that entered into the crystal lattices of TiO2 led to the formation of defects in the crystal lattices of TiO2 and thereby improved the photocatalytic activity of TiO2.When WO3 doped in TiO2 exceeded 3%, the excess W^6＋ did not enter into the crystal lattices of TiO2 but were uniformly dispersed in TiO2 or they covered the surface of TiO2, which reduced the effective illumination area of TiO2 and thereby lowered the photocatalytic activity of TiOE.The relationship among the composition of the catalyst, the amount of photocatalyst, the illumination time, and the decolorizing rate of methyl orange （MO） were discussed. The results show that the decolorizing rate of MO can reach 82.3% using WO3/TiO2 as the photocatalyst, with the composition of WO3/TiO2 -3：97, the mass of catalyst = 0.400 g, the initial concentration of MO = 20 mg/L, pH = 6.5, and the illumina- tion time = 7 h.     

均分散球形Y2O3：Eu^3＋纳米晶的制备

采用凝胶网格共沉淀法，以明胶为反应基质制备了单分散球形纳米Y2O3：Eu^3 荧光粉，考察了制备条件对产物粒径的影响。利用X射线衍射(XRD)、透射电子显微镜(TEM)和荧光光谱等手段对样品进行了表征。结果表明：该法制得产物为球形，一次晶粒粒径在13nm～25am之间，且粒度分布均匀，与微米晶相比，该纳米晶的激发光谱发生明显红移。