掺杂稀土铁磁性纳米复合粉体的制备

采用水热法以FeCl2和KOH为原料制备Fe3 O4粉体,以氧化钇、氧化铕和氧化铽为原料制备Y2 O3:1;Eu3+,5;Tb3+粉体,然后以Fe3 O4粉体,Y2 O3:1;Eu3+,5;Tb3+粉体和三聚氰胺为原料,采用微波烧结法在Ar气气氛下制备FeYO3/Y2 O3:1;Eu3+,5;Tb3+复合粉体,利用XRD衍射仪对各种粉体的结构进行分析,利用扫描电镜对复合粉体的形貌进行观察,并利用振动样品磁强计对复合粉体的磁学性能进行研究.结果表明:复合粉体均呈针状,长度和细度均为纳米级.当Fe3 O4,Y2 O3:1;Eu3+,5;Tb3+和三聚氰胺比例为1:3:4时,所制备的FeYO3/Y2 O3:1;Eu3+,5;Tb3+粉体磁力最强,磁力饱和强度为11.3 emu·g-1.     

碳酸盐沉淀法合成Nd3+:Y2O3激光陶瓷纳米粉体

以Y2O3粗粉、Nd2O3、硝酸和NH4HCO3为原料,通过共沉淀法制备了Nd3+:Y2O3透明激光陶瓷纳米粉体,并采用TG/DTA、XRD、FTIR、TEM以及EDS等测试方法对粉体性能进行了表征.结果表明,在先驱物中添加适量SO42-离子能减轻煅烧得到的Nd3+:Y2O3粉体的团聚,使粉体粒度均匀并呈球形分布.在1100 ℃煅烧4 h所得粉体粒度均匀,粒径在50～70 nm之间,具有较好的分散性,适合作为制备透明激光陶瓷的粉体材料.     

单一基质Na2Ca3Si2O8∶Tb3+,Eu3+荧光粉发光性质和能量传递的研究

通过传统的高温固相法成功的制得了一系列紫外激发的硅酸盐荧光粉Na2 Ca3 Si2O8∶Tb3+,Eu3+.X射线衍射(XRD)研究表明所制得的荧光粉为纯相.在Na2Ca3Si2O8∶Tb3+,yEu3+荧光粉体系中,随着Eu3+的掺杂浓度增大,发射光谱中Tb3的特征峰发光强度降低而Eu3+的不断升高,并且荧光寿命不断减小,说明了Tb3+和Eu3之间能量传递方式是交换相互作用,能量传递效率(ET)达到了15.8;.此外,通过CIE色坐标观察到,随着Eu3+浓度的增加,样品从绿色变成黄色,最终变成红色.由于它多彩的颜色变化,所以它是一种用于制作多彩LED的良好材料.     

沉淀法制备(Eu0.045Li3xNa3yGdz/Luw)2O3纳米晶及发光性能研究

采用沉淀法制备了(Eu0.045Li3xNa3yGdz)2O3和(Eu0.045Li3xNa3yLuw)2O3纳米晶,通过测量粉体的XRD、SEM、激发谱、发射谱,讨论了不同比例阳离子合成样品的发光特性.实验表明,800℃下,Eu3+、Li+、Na+完全掺入G2O3和Lu2O3晶格,且对基质立方相无影响;添加了碱金属锂、钠离子的样品,晶粒生长更完善;对于氧化钆基质,Eu3+、Li+、Na+、Gd3+比例为4.5:4:4:87.5(摩尔百分比)时,样品发光比不掺碱金属锂、钠离子的样品发光提高6倍;对于氧化镥基质,Eu3+、Li+、Na+、Lu3+的摩尔百分比为4.5: 1:1:93.5时,样品比不掺碱金属锂、钠离子的样品发光提高约4倍.     

Y2O3∶Yb3+,Tm3+纳米粉体的制备及发光性能研究

以Y2O3为基质材料,Yb3+为敏化剂,Tm3+为激活剂,采用化学共沉淀法制备Y2O3∶Yb3+,Tm3+纳米粉体,通过差热、红外光谱、XRD、荧光、上转换发光和场发射电子显微镜等方法对样品进行表征.结果表明:Tm3+和Yb3+完全固溶到Y2O3立方晶格中,且粉体大小均匀,尺寸约50 nm;Yb3+浓度为4;(摩尔分数)、煅烧温度900 ℃时,荧光和上转换发光强度最强;Tm3+浓度为0.4;时绿光(5F4/5S2→5I8)和红光(2F5/2→2F7/2)荧光强度最强,浓度0.5;时蓝光(1G4→3H6)和红光(1G4→3F4)的上转换发射强度最大.     

微波法制备CaMoO4:Tb3+,Eu3+白色荧光粉及其发光性能研究

通过微波法制备了CaMoO4:Tb3+,Eu3+白色荧光粉.采用X射线粉末衍射仪、扫描电子显微镜和荧光光谱仪对样品材料的结构、形貌和发光性能进行了表征.分别讨论了在不同助剂、不同反应浓度、不同反应温度及稀土离子Eu3+和Tb3+共掺比例变化对荧光粉的发光性能的影响.结果表明:不加活性剂所得CaMoO4:Tb3+,Eu3+样品在反应浓度为0.06 mol/L、反应温度为120℃时发光性能最好;通过调节CaMoO4:Tb3+,Eu3+荧光粉中稀土离子Eu3+和Tb3+共掺比例荧光粉的发光颜色可以很容易地从冷白光变为暖白光.     

近紫外光LED芯片用红色荧光粉SrIn2O4∶Eu3+,Sm3+的制备及性能研究

利用高温固相法制备了EH3+、Sm3单掺杂及共掺杂的SrIn2O4荧光材料.通过XRD、激发光谱、发射光谱等对SrIn2O4∶ Eu3+、SrIn2O4∶ Sm3+、SrIn2O4∶ Eu3+,Sm3+进行表征.结果表明,SrIn2O4∶ Eu3+在近紫外光395 nm激发下能够有效的产生616 nm的红光发射.在SrIn2 O4∶Sm3+体系中发现,该系列样品适合于407 nm的紫光激发,发射峰位于607 nm.在SrIn2O4∶Eu3+,Sm3+体系中,通过光谱分析发现,基质中存在Eu3和Sm3激活剂之间的相互能量传递过程.该能量传递过程使SrIn2O4∶Eu3+,Sm3+更适合于390～410 nm紫外芯片激发的LED用红色荧光粉.     

碳酸盐沉淀法合成Nd^3＋：Y2O3激光陶瓷纳米粉体

以Y2O3粗粉、Nd2O3、硝酸和NH4HCO3为原料,通过共沉淀法制备了Nd^3＋：Y2O3透明激光陶瓷纳米粉体,并采用TG／DTA、XRD、FTIR、TEM以及EDS等测试方法对粉体性能进行了表征。结果表明,在先驱物中添加适量SO4^2-离子能减轻煅烧得到的Nd^3＋：Y2O3粉体的团聚,使粉体粒度均匀并呈球形分布。在1100℃煅烧4h所得粉体粒度均匀,粒径在50～70nm之间,具有较好的分散性,适合作为制备透明激光陶瓷的粉体材料。     

海胆状Eu2O3/Ag3VO4复合材料的水热合成及其光致发光性能

以硝酸银和氧化铕为金属源,P123为结构导向剂,乙醇和水为溶剂.本文通过前驱体合成路线,采用水热法得到海胆状Eu2 O3/Ag3 VO4微球,并探讨其合成条件;采用SEM、XRD、XPS等方法对样品进行了表征,并探讨了Eu2 O3/Ag3 VO4海胆状微纳米结构的形成过程.测试结果表明:在反应温度为80℃,反应时间为10 h时,所合成的海胆状Eu2 O3/Ag3 VO4微球直径约为4~5μm.针对合成的样品,研究了海胆状Eu2 O3/Ag3 VO4微球的光致发光性能,并考察Eu3+掺杂量对光致发光性能的影响,当Eu3+掺杂量为4;时,样品具有最好的光致发光性能.     

LaP3O9∶Eu3+荧光粉的制备及发光性能研究

以La2O3、Eu2O3和(NaPO3)6为原料,采用共沉淀法制备了LaP3O9∶Eu3+荧光粉,并对其发光性能进行了分析。结果表明:该荧光粉的最强吸收峰位于391 nm处;两个发射峰分别位于587 nm和616 nm处,且两峰发光强度相近,说明Eu3+在LaP3O9∶Eu3+晶体场中处于具有非反演中心对称的格位;与LaPO4∶Eu3+荧光粉相比LaP3O9∶Eu3+发出的红光色饱和度更高;Eu3+在LaP3O9∶Eu3+晶体荧光粉中的掺杂浓度为8at%时,发光强度最大。     

Synthesis of spindle‐shaped α‐FeOOH and α‐Fe2O3 nanocrystals

Spindle‐shaped α‐FeOOH nanocrystals were facilely synthesized using a poly (vinyl pyrrolidone) (PVP)‐assisted route under hydrothermal conditions. The chemical compositions and morphol‐ogies of the as‐prepared samples were characterized in detail by X‐ray power diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscope (TEM). The experimental results reveal that these spindle‐shaped α‐FeOOH nanocrystals have self‐organized into assemblies with hierarchical nanostructures. The crucial roles of PVP in the hydrothermal synthesis of hierarchical α‐FeOOH nanostructures were discussed. The possible formation mechanism was also suggested. Moreover, the spindle‐shaped α‐Fe₂O₃ nanocrystals could be easily obtained after calcining the α‐FeOOH prepared by the PVP‐assisted hydrothermal process. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Geometric modeling of homoepitaxial CVD diamond growth: I. The {1 0 0}{1 1 1}{1 1 0}{1 1 3} system

Plasma-assisted CVD homoepitaxial diamond growth is a process that must satisfy many stringent requirements to meet industrial applications, particularly in high-power electronics. Purity control and crystalline quality of the obtained samples are of paramount importance and their optimization is a subject of active research. In the process of such studies, we have obtained high purity CVD diamond monocrystals with unusual morphologies, namely with apparent {1 1 3} stable faces. This phenomenon has led us to examine the process of CVD diamond growth and build up a 3D geometrical model, presented here, describing the film growth as a function of time. The model has been able to successfully describe the morphology of our obtained crystals and can be used as a predictive tool to predetermine the shape and size of a diamond crystal grown in a given process configuration. This renders accessible control of desirable properties such as largest usable diamond surface area and/or film thickness, before the cutting and polishing manufacture steps take place. The two latter steps are more sensitive to the geometry of the growth sectors, which will be addressed in a companion paper.Our model, applicable to the growth of any cubic lattice material, establishes a complete mapping of the final morphology state of growing diamond, as a function of the growth rates of the crystalline planes considered, namely {1 0 0}, {1 1 1}, {1 1 0}, and {1 1 3} planes, all of which have been observed experimentally in diamond films. The model makes no claim as to the stability of the obtained faces, such as the occurrence of non-epitaxial crystallites or twinning. It is also possible to deduce transient behavior of the crystal morphology as growth time is increased. The model conclusions are presented in the form of a series of diagrams, which trace the existence (and dominance) boundaries of each face type, in presence of the others, and where each boundary crossing represent a topology change in terms of number of faces, edges and vertices. We validate the model by matching it against crystals published in the literature and illustrate its predictive value by suggesting ways to increase usable surface area of the diamond film.     

synthesis of high‐quality crystalline α‐MoO3 nanobelts

High‐quality crystalline MoO₃ nanobelts were successfully fabricated with a facile hydrothermal route by using common and inexpensive NaCl as a capping agent. The products are thoroughly characterized by the combination of different techniques. The results indicate that as‐prepared MoO₃ nanobelts have an orthorhombic crystal structure (α‐MoO₃) with growth preferential in the [001] direction, the size of the obtained MoO₃ nanobelts ranges from 200 nm to 300 nm in width and micrometers in length. The effects of the amount of NaCl on the morphology and size of the resultant MoO₃ were also investigated, it is clearly shown that the presence of appropriate amount of NaCl plays a crucial role in controlling the size and morphology of the obtained MoO₃. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Crystal and Molecular Structure of 6α-Methyl-3,20-Dioxo-5β-Pregnan-17α-yl Acetate

The title compound 6α-methyl-3.20-dioxo-5β-pregnan-17α-yl acetate crystallizes in the monoclinic space group P 2₁ with two molecules in the unit cell and the lattice parameters a = 10.889, b = 11.056, c = 9.8029 Å, β = 101.51° The crystal structure is isostructural with medroxyprogesterone acetate and refined by full matrix least squares calculations up to the discrepancy factor R = 0.051.     

The crystal and molecular structure of 5α,8α-epidioxyergosta-6,22-dien-3β-acetate

From the mushroom species Tricholoma populinum LANGE which shows interesting pharmaceutical effects the steroid 5α,8α-epidioxyergosta-6,22-dien-3β-ol has been isolated. The acetate of this compound crystallizes in the monoclinic space group P 2₁ with two molecules in the unit cell of dimensions a = 19.788, b = 7.241, c = 9.914 Å, β = 103,97°. The final R-value is 0.079 for 1082 reflections.     

Characterization of α and γ polymorphs of glycine crystallized from water‐ammonia solution

Crystallization of metastable α and stable γ polymorphs of glycine was carried out from aqueous solution in the presence of ammonia. Pure aqueous solution and solution with lower concentration of ammonia yield α nucleation and solution with a critical concentration of ammonia yield γ nucleation. Variation in the solubility of glycine in double distilled water and pH of the resulting solution due to the ammonia incorporation was studied in a range of temperatures. The induction period for the α and γ nucleation in the solution was determined and its variation due to the ammonia incorporation was also studied. Single crystals of both the polymorphs were grown by slow evaporation method. Effect of ammonia concentration and the resultant pH of the solution on the nucleation, growth and morphology of the grown polymorphs were investigated. The unidirectional growth of the γ polymorph along the polar axis was revealed. X‐ray powder diffraction method was employed to distinguish both the polymorphs structurally. Their thermal stability above room temperature was studied by differential scanning calorimetry which revealed that the as‐grown γ polymorph transforms to α at 179.6 °C while the as‐grown α retains its phase until melting. The optical transmittance of the grown γ polymorph was studied in the UV‐Vis‐Near IR region. The second harmonic generation (SHG) efficiency of the grown γ polymorph was studied with a Nd:YAG laser source and is about 6.8% higher than that of the inorganic standard KDP. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The Crystal and Molecular Structure of 1α,2α-Methylene Gibberellin A3 Methyl Ester

The three-dimensional structure of the 1α,2α-methylene gibberellin A₃ methyl ester has been determined by single-crystal X-ray diffraction techniques. The crystals are monoclinic, space group P 2₁ with two molecules in the unit cell of dimensions a = 9.236, b = 7.109, c = 14.155 Å and β = 104.61º. The structure was refined to an R-value of 0.0983 for 1359 observed reflections.     

Effective electro‐optic coefficient of (1–x)Pb(Zn1/3Nb2/3)O3–xPbTiO3 single crystals

Refractive indices and effective electro‐optic coefficient γ_c of (1–x)Pb(Zn_1/3Nb_2/3)O₃–xPbTiO₃ (PZN‐xPT, x = 0.05, 0.09 and 0.12) single crystals were measured at 532 nm wavelength. Orientation and temperature dependences of the electro‐optic coefficient were investigated. Large electro‐optic coefficient (γ_c = 470 pm/V) was observed in [001]‐poled PZN‐0.09PT crystal. More importantly, γ_c of tetragonal PZN‐0.12PT is almost unchanged in a temperature range −20 ∼ 80 °C. The γ_c of PZN‐xPT single crystals are much higher than that of widely used electro‐optic crystal LiNbO₃ (γ_c = 20 pm/V). These results show that PZN‐xPT single crystals are very promising materials for electro‐optic modulators in optical communications.     

3 β ‐Acetoxy‐5 α ‐cholestan‐6‐one: A Steroid

The crystal and molecular structure of 3 β ‐Acetoxy‐5 α ‐cholestan‐6‐one has been determined by X‐ray crystallographic techniques. The compound crystallizes in the space group P2₁ with cell parameters : a = 13.060(3), b=6.299(2), c=17.152(6)Å; β =96.47(3)o, V = 1402.02ų, Z = 2, R = 0.072 for 1921 observed reflections. The six‐membered rings (A, B and C) exist in the chair conformations while the five‐membered ring‐d assumes half‐chair. All rings of the steroid skeleton are trans connected.     

Synthesis and properties of α‐Fe2O3 nanorods

We report synthesis of α‐Fe₂O₃ (hematite) nanorods by reverse micelles method using cetyltrimethyl ammonium bromide (CTAB) as surfactant and calcined at 300 °C. The calcined α‐Fe₂O₃ nanorods were characterized by X‐ray diffraction (XRD), high‐resolution scanning electron microscopy (HRSEM), transmission electron microscopy (TEM), energy dispersive spectrometer (EDS), fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer (VSM). The result showed that the α‐Fe₂O₃ nanorods were hexagonal structure. The nanorods have diameter of 30‐50 nm and length of 120‐150 nm. The weak ferromagnetic behavior was observed with saturation magnetization = 0.6 emu/g, coercive force = 25 Oe and remanant magnetization = 0.03 emu/g. (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)