微乳液电纺丝法制备Eu3+掺杂锆酸镧多孔纤维及其发光性能研究

以LaCl₃、ZrClO₂·8H₂O为原料,无水乙醇为溶剂,采用微乳液静电纺丝法制得烧绿石型的锆酸镧纤维,并引入分相剂石蜡在纤维中构筑多孔结构.采用XRD、SEM和BET研究了纤维的结构和形貌,采用PL光谱测试了Eu³⁺掺杂的锆酸镧纤维的发光性能.研究表明,引入分相剂石蜡可以改善纤维中的孔结构,当石蜡用量为4 mL时所制备的锆酸镧纤维物相纯度高,其比表面积为20.77 m²·g^-1,平均孔径19.3 nm,有较为丰富的孔结构且分布均匀.因此,在该纤维中掺杂Eu³⁺后,由于氧离子与稀土离子间的电荷跃迁,以及多孔结构光散射的作用,多孔纤维的发光强度有所提高.     

微乳液静电纺丝制备多孔Nb4N5纤维及其电化学性能

以五氯化锯为原料,液体石蜡为分相剂,采用微乳液静电纺丝技术制备前驱体纤维,再经氨气还原氮化得到多孔氮化锯纤维.利用XRD、SEM、BET等进行物相及微观结构表征,结果表明合成的纤维为四方Nb4N5晶相,纤维连续,直径为260 nm,由于液体石蜡分相以及助纺剂PVP的分解作用,在纤维上形成较多孔道结构,其BET比表面积为125m2/g,孔径为2～5nm范围内的孔结构比例较高,同时在5～10 nm 范围也存在较多的孔道结构,平均孔径为7.3 nm.采用CV、GCD及EIS等测试其电化学性能发现,氮化锯纤维的储能主要受电极表面电荷传递过程控制的,外表面比电容贡献高,这得益于分布在纤维中的孔结构,其可为离子传输提供通道,并为电化学反应提供空间.当电流密度为5mA/g时,比电容为151 F/g,能量密度为7.73 Wh/kg时,功率密度为3.03 W/kg,其经2000次循环后其比电容保持在95;以上.     

多孔氧化铝模板电沉积法制备ZnO纳米结构阵列的研究

利用直流电化学沉积技术,在多孔氧化铝模板内,通过先沉积Zn(OH)2/ZnCO3,然后在300℃下进行热分解,制得了ZnO纳米点阵结构.扫描电镜结果表明多孔氧化铝模板孔道呈六角形分布,孔径约为55 nm,孔间距约为100 nm,且孔道上下贯通平行排列.X射线衍射表明多孔氧化铝模板为非晶结构,孔内组装的ZnO具有多晶纤锌矿结构.光致发光谱表明ZnO/PAM复合体系同空氧化铝模板相比在420 nm处具有较强的蓝光发射.     

电气石对硅藻土基多孔陶瓷孔结构与孔雀石绿脱色效果的影响

以硅藻土为主要原料,采用固相烧结法和低温煅烧工艺,制备了硅藻土基多孔陶瓷.着重考察了电气石对材料的微观结构、孔径分布等材料孔结构及孔雀石绿溶液脱色能力的影响,通过扫描电镜、压汞仪等手段对不同电气石含量的硅藻土基多孔陶瓷进行了表征.结果表明:当电气石含量为12;时,材料内孔径细小,平均孔径最小177.5 nm,比表面积最大6.83 m2/g;电气石含量由0提高到16;,材料的孔隙率由49.3;降至36.5;,对孔雀石绿溶液的脱色能力逐渐增强.当电气石含量为16;时,反应6 h后,412 nm与618 nm处吸收峰消失.     

纳米微结构材料多孔氧化铝膜的制备及应用

本文简要地介绍了多孔氧化铝理论模型的发展历程,采用目前较为成熟的阳极氧化法制备有序多孔氧化铝薄膜.讨论了多孔氧化铝自身的物理性质,重点展示了如何充分利用多孔氧化铝作为模板制备纳米材料的美好前景,明确了今后的工作重点为开拓新的应用领域及对多孔氧化铝膜孔径大小及孔的形状进行有效控制.     

不同粒度的Fe2O3对堇青石蜂窝陶瓷性能的影响

以高岭土、滑石粉、工业氧化铝和不同粒度的Fe2O3粉为原料,研究了Fe2 O3粉的粒度对堇青石蜂窝陶瓷相组成、微观形貌和孔径分布的影响.实验结果表明:随着外加Fe2O3粉粒度的减小,加快了离子扩散速率,固溶量增加,堇青石的固相反应速率增加.当Fe2O3粉粒度为5μm和50μm时试样的微观结构中有微裂纹产生,为降低材料的热膨胀系数打下了基础.随着加入Fe2O3粉粒度的逐渐增大,产生液相,填充了试样中微孔,使孔径尺寸减小,孔径数量减少.     

TBA/H2O溶液冷冻干燥制备多孔Al2O3支架及其生物性能

以叔丁醇/蒸馏水(TBA/H2O)结晶体为模板,用冷冻干燥法制备出片层孔及圆形孔的两种孔型氧化铝支架材料,利用SEM观察支架形貌,测试了其生物性能,系统研究浆料溶剂组分含量、冷冻温度对支架材料形貌影响,探讨支架孔结构对成骨细胞附着的影响.结果表明:纯水浆料的多孔陶瓷支架形貌为片层状;加入叔丁醇后,片层间距减少;浆料中叔丁醇含量为90wt;时,孔道呈片层孔及圆形孔的双孔状;纯叔丁醇浆料的陶瓷支架形貌为圆形孔.双孔形貌支架的开孔孔隙率及总孔隙率最高,分别为78.5;和81.8;.孔径随冷冻温度的降低而减小.体外模拟实验表明:片层孔及圆形孔的双孔支架材料有利于细胞在其表面生长,材料表面细胞结构清晰,铺展形态良好.多孔支架材料对细胞的吸附率随孔径的增大而增大.冷冻温度为-10℃时,支架的压缩强度为90.6 MPa,符合骨组织工程中支架材料的强度值要求.     

AAO纳米光栅结构参数对薄膜硅太阳能电池光吸收的影响研究

以多孔氧化铝(AAO)为模板设计了一种新型的纳米光栅背反射结构.采用微波工作室(CST MWS)软件对该结构进行仿真,研究AAO模板的孔径大小、孔径深度和占空比对薄膜硅太阳能电池光吸收的影响.仿真结果表明,以AAO为模板制备的新型背反射结构能够有效地延长光的传播路径,增加长波长光子的吸收.当孔径大小为157.2 nm,孔深为78.6 nm,占空比为0.5时,效果最佳.这与理论的计算结果相一致.     

低温燃烧-烧结法制备多孔Al2O3/ZrO2(Y2O3)陶瓷

用低温燃烧合成的陶瓷粉体为原料,在1450℃下烧结制备了多孔Al2O3/ZrO2 (3mol; Y2O3)陶瓷,并研究ZrO2的外加量(Omol;、1Omol;、15mol;和20mol;)对多孔陶瓷显气孔率、抗弯强度、孔径分布和显微结构的影响.实验结果表明:与其他试样相比,ZrO2外加量为15mol;的试样的显气孔率和抗弯强度都明显提高,其最可几孔径约为1.1 μm.SEM和EBSD图片显示:外加ZrO2能显著影响多孔陶瓷的显微结构,其中外加15mol; ZrO2的多孔陶瓷中,氧化铝晶粒的平均尺寸较小,颈部较厚,这是其具有较高抗弯强度的主要原因.     

双模板法制备分级孔结构SiC陶瓷

以冰晶和聚苯乙烯(PS)微球为模板,微米级SiC粉体为原料,通过双模板法制备了具有三级孔径分布的多孔SiC陶瓷.研究了SiC的固含量和PS微球的大小对多孔SiC陶瓷的微观形貌、孔隙率和压缩强度的影响.研究结果表明:分级孔结构的多孔SiC陶瓷具有冰模板升华后遗留下的对齐排列的大孔、分布于孔壁中的由PS微球热解留下的中孔和颗粒之间堆积形成的小孔.随着SiC固相含量的增加,大孔孔径和孔容降低,但压缩强度增加.当PS微球粒径约为0.90 μm时,中孔孔径分布在0.7～1.5 μm之间;当PS微球粒径约为2.51 μm时,孔径分布较宽,约为1～3 μm.     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Crystal structures of the cis and trans isomers of a tetrathia[3.3.3.3]cyclophane

Both the cis and trans isomers of 3,11,18,26-tetrathiatricyclo[26.2.2.1^5,9.2^13,16.1^20,24] hexatriaconta-5,7,9,20,22,24-hexene have been prepared and structurally characterized. Each of these centrosymmetric tetrathia dimers includes two cyclohexane rings in chair conformations with either 1,4-cis or 1,4-trans bonding and two meta-substituted benzene rings. The cis isomer packs into the monoclinic space group P2₁/a with a = 10.485(3)Å, b = 10.3956(18)Å, c = 14.1343(10)Å, = 105.200(13)°, Z = 2 and refined to an R factor of 0.046. The trans isomer crystallizes in the monoclinic space group P2₁/c with a = 10.7217(12)Å, b = 5.6797(7)Å, c = 25.415(5)Å, = 96.001(12)°, Z = 2 and refined to an R factor of 0.043. In the cis structure each benzene ring faces a cyclohexane ring while in the trans structure the cyclohexane rings face one another.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

电沉积法制备ZnO纳米棒阵列及其发光特性

本文以掺F的SnO2导电玻璃为基板,以硝酸锌水溶液为电解液,采用三电极恒电位体系电沉积制备ZnO纳米棒阵列,系统考察了硝酸锌浓度和沉积电位等工艺参数对ZnO纳米棒阵列的微观形貌及其发光性能的影响规律.结果表明,硝酸锌浓度和沉积电位对纳米棒阵列的形貌有显著影响,控制适宜的工艺条件可以制备出直径分布均匀、结晶性好且纯度高的六方纤锌矿ZnO纳米棒阵列.荧光光谱分析表明,电沉积制备出的ZnO纳米棒阵列在385 nm附近有一个强荧光发射峰,且发光性能稳定、对纳米棒阵列微观形貌的细微变化不敏感,使其在发光二极管和激光器等领域具有广阔的应用前景.