氩氧流量对ZAO薄膜微结构及其光学性能影响

运用射频磁控溅射技术,改变氩氧流量比在玻璃衬底上生长ZnO∶ Al(ZAO)样品,采用XRD、紫外-可见分光光度计对薄膜微结构、厚度及其光学性能表征,结果发现:维持氩流量不变(9 sccm),随着氧流量增加(1～9 sccm),样品XRD峰强减小,半高宽增大,晶粒尺寸减小,薄膜结晶性能变差;而维持氧流量不变(9 sccm),氩流量减小(9～3 sccm),样品XRD峰强增大,半高宽减小,晶粒尺寸变大,结晶性能变好.紫外可见光光谱在400 ～ 900nm波长区间平均透射率差异大(67.9; ～91.1;);在420 ～ 900 nm波长区间平均透光率高且差异小(90.2; ～92.4;).     

氮流量对ZnO∶N薄膜微结构及光学性能影响

运用射频磁控溅射技术,改变氩、氮流量比(9/1 ～ 9/4)在玻璃衬底上获得ZnO∶N样品,采用XRD、紫外-可见分光光度计、傅里叶红外光谱仪及SEM对薄膜微结构和光学性能表征.结果发现∶N流量小,样品XRD峰强小,峰位不明显,紫外可见光光谱在320 ～780 nm波长区间透射率变化小;随着N流量的增加,样品XRD有(002)强单峰出现,在400 nm波长以下透射率急剧下降;当氩氮流量达到9/4,样品XRD出现双峰,紫外光透射率无明显变化.     

Ag掺杂ZnO薄膜结构和光学特性研究

采用脉冲激光沉积技术制备出了Ag掺杂的ZnO薄膜.研究了Ag含量、衬底温度及氧压对ZnO结构和光学性能的影响.结果表明:Ag以替位形式存在于ZnO晶格中,Ag掺杂浓度较低时,样品具有高度c轴择优取向.衬底温度越高,薄膜的结晶质量越好,光学带隙越接近纯ZnO的带隙,而其紫外荧光峰在衬底温度为300 ℃时最强.氧压为10 Pa时,薄膜的结晶质量最好,紫外峰最强,其带隙则随氧压的增大呈先变窄后加宽的趋势.     

Na掺杂ZnO薄膜的表面形貌及其光学性质

采用溶胶-凝胶技术制备不同Na掺杂ZnO薄膜,用XRD、拉曼光谱仪、AFM、SEM和紫外可见分光光度计等表征方法研究了Na掺杂量对ZnO薄膜的表面形貌和光学性质的影响.XRD和Raman光谱分析表明:8.0 at;Na掺杂ZnO薄膜具有最佳c轴择优取向,内部残余张应力最大;表面形貌研究结果显示:薄膜的平均粒径和粗糙度均随Na含量的增加而增大.薄膜在可见光范围内的平均透射率大于80;,随着Na含量从0增加到10at;,薄膜的光学带宽由3.283 eV增大到 3.305 eV.     

磷扩散法制备高掺磷p型ZnO薄膜的磁控溅射工艺的探索

在前期通过n+-Si衬底中的磷向沉积于其上面的ZnO薄膜的扩散制备高掺磷p型ZnO薄膜的研究基础上,探索了较有普遍应用意义的扩散法制备p型ZnO薄膜的磁控溅射工艺.结果表明,当磁控溅射的氧氩质量流量比与衬底温度满足特定的低阶指数函数的匹配关系时,所制备的ZnO薄膜为p型,而且薄膜中磷原子的深度分布是均匀的;另外,这种薄膜的厚度随着氧氩流量比的增加而减小,而薄膜中氧锌原子浓度比都大于1,比值大小与氧氩质量流量比和衬底温度有关.     

Ti含量对溶胶-凝胶法制备Ti、Ga共掺ZnO薄膜性能的影响

采用溶胶-凝胶旋涂法在玻璃衬底上沉积纳米结构Ti、Ga共掺ZnO薄膜(TGZO,Ga掺杂量为1.0;(原子分数,下同)),用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、分光光度计(UV-Vis)、四探针测试仪、霍尔效应测试仪研究了Ti含量对TGZO薄膜的物相组成、表面形貌、电学和光学性能的影响.结果表明:所有TGZO薄膜均表现出六方纤锌矿的多晶结构,并具有(002)择优取向生长,在380～780 nm波长范围内具有良好的透射率(>86;);随着Ti含量的增加,TGZO薄膜的晶粒尺寸和可见光平均透射率均先增加后减小,而光学带隙和电阻率先减小后增加;Ti掺杂量为1.0;时,具有最高的可见光透射率92.82;,最窄的光学带隙3.249 eV,以及最低电阻率2.544×10-3Ω·cm.     

PET上沉积Al掺杂ZnO薄膜的光电特性研究

采用脉冲激光沉积技术(PLD),室温下在柔性衬底PET上制备了高度c轴择优取向的Al掺杂ZnO薄膜.XRD分析表明,不同Al掺杂浓度的样品均呈现单一的ZnO相.荧光光谱和透射光谱分析显示,低温低氧压下制备的Al掺杂ZnO薄膜在紫光区域有很强的荧光发射,在可见光区域具有较高的透射率;并且可以通过Al掺杂浓度调节薄膜紫色发光强度和薄膜带隙.薄膜的电阻率随着Al掺杂浓度的增加先降低后增加,在掺杂浓度为3;原子分数时达到最小值.     

溅射功率对硫化镉薄膜结构和光电性能的影响

在玻璃衬底上采用射频磁控溅射方法制备了硫化镉(CdS)薄膜,研究了溅射功率对CdS薄膜的结构、表面形貌、光学特性和电学性质的影响.XRD测量表明制备的CdS薄膜均为六方纤锌矿结构的多晶薄膜.随着功率从40 W增加到80 W,H(102)面的峰呈现增强再逐渐减弱的趋势.60 W时薄膜的衍射峰最强,结晶度最好.同时,薄膜的晶粒尺寸随着功率增加先增大再减小.从SEM图像可以看出,制备的薄膜均匀致密且无针孔的出现.在可见光范围内,薄膜的平均透射率都在70;以上.随着功率的增加,薄膜带隙在2.25～2.41 eV的范围内变化,而暗电导率呈现先增加再减少的趋势.     

Nb掺杂ZnO透明导电薄膜的结构以及光电性能研究

采用直流磁控溅射法在玻璃衬底上制备了高质量的Nb掺杂ZnO( NZO)透明导电薄膜.为了研究薄膜厚度对薄膜性质的影响,制备了五个厚度分别为239 nm,355 nm,489 nm,575 nm和679 nm的样品.XRD结果表明,ZnO∶ Nb薄膜是具有六角纤锌矿结构的多晶薄膜,并且具有垂直于衬底的c轴择优取向.随着膜厚的增加,薄膜的结晶质量明显提高.当厚度从239 nm增加到489 nm时,平均晶粒尺寸从19.7 nm增加到24.7 nm,薄膜的电阻率持续减小;当厚度进一步增加时,晶粒尺寸略有减小,电阻率有所增加.本实验获得的最低电阻率为4.896×10-4Ω·cm.随膜厚的增加,光学带隙先增大后减小.所有薄膜在可见光区域的平均透过率均超过88.3;.     

B掺杂对平面结构MOCVD-ZnO薄膜性能的影响

本文研究了B2H6掺杂流量(B掺杂)对平面结构MOCVD-ZnO薄膜的微观结构和光电性能影响.XRD、SEM和AFM测试的研究结果表明,玻璃衬底上制备的ZnO薄膜具有(002)峰择优取向的平面结构,B掺杂使薄膜的球状晶粒尺寸变小,10 sccm流量时晶粒尺寸为～15 nm.ZnO:B薄膜的最小电阻率为5.7×10-3Ω·cm.生长的ZnO薄膜(厚度d=1150 nm)在400～900 nm范围的透过率为82;～97;,且随着B2H6掺杂流量增大,光学吸收边呈现蓝移(即光学带隙Eg展宽)现象.     

CsI-LiCl共晶材料的坩埚下降法生长与闪烁性能研究

本文采用坩埚下降法,在真空密封的石英坩埚中成功生长出CsI-LiCl与CsI-LiCl:Na共晶闪烁体。通过扫描电子显微镜(SEM)观察晶体微结构表明该共晶中LiCl相与CsI相存在周期性的层状排列,CsI相的厚度在5 μm左右。共晶样品的X射线激发发射谱显示在CsI-LiCl和CsI-LiCl:Na共晶样品存在缺陷发光,在CsI-LiCl样品中还观察到了纯CsI的自陷激子(STE)发光。CsI-LiCl样品在α粒子激发下的多道能谱中观察到明显的全能峰,这一结果证明CsI-LiCl共晶可用于热中子探测的潜力。     

静电纺丝法制备CeO2微纳米纤维及其除氟性能

以聚丙烯腈(PAN)为载体,六水合硝酸铈[Ce(NO₃)₃·6H₂O]为原料,采用静电纺丝法制备了Ce(NO₃)₃/PAN纤维,在空气中热处理得到CeO₂微纳米纤维,通过XRD、BET和SEM对CeO₂微纳米纤维进行表征。采用静态吸附实验探讨了CeO₂微纳米纤维去除水溶液中氟离子的性能,考察了溶液pH值、初始氟离子浓度及共存阴离子等对吸附性能的影响。结果表明,pH=3时,CeO₂微纳米纤维对F^-的吸附性能最佳,CeO₂吸附量随着F^-浓度的增大呈上升趋势。CeO₂微纳米纤维对F^-的吸附等温线遵循Langmuir模型,二级动力学模型能很好地描述CeO₂微纳米纤维对F^-的吸附过程。CeO₂微纳米纤维的除氟性能优良,可为其实际应用提供理论参考。     

Selinidin: Crystal structure generated by C–H···O, C–H···π and π-π interactions

The title compound, 9,10-dihydro-8,8-dimethyl-2-oxo-2H,8H-benzo[1,2-b:3,4-b']dipyran-9-yl-2-methyl-2-butenoate, C₁₉H₂₀O₅, was isolated from the roots of Selinum vaginatum. The compound crystallizes into monoclinic space group P2 ₁ with unit cell parameters: a = 12.830(2) Å, b = 9.041(1) Å, c = 14.983(1) Å, β = 95.09(1)°, Z = 4. The crystal structure has been determined using direct methods and refined by full-matrix least-squares to a final R value of 0.0529 for 3142 observed reflections. There are two independent molecules, A and B, per asymmetric unit. In both the molecules, the coumarin nucleus is planar. However pronounced differences are observed in the conformation of dihydropyran ring which has a half-chair conformation with an 8β-9α orientation in molecule A and is intermediate between half-chair and sofa in molecule B. Differences also occur in the conformation of the 2-methylbutenoyloxy side chain at C9 due to the different geometry of C–H···π interactions in molecules A and B. Molecules A and B are connected by π–π interactions between their coumarin fragments forming dimers. The dimers interact through C–H···O and C–H···πhydrogen bonds.     

Chromene and Imidazole Based D-π-A Chemosensor Preparation and Its Anion Responsive Effects

We have designed and synthesized the colorimetric chemosensor through the reactions of 2-(4H-chromen-4-yildene)malonitrile and 4-imidazolecarboxaldehyde. Due to its well conjugated D-π-A system and the existence of NH- fragment in structure, we expected that the chemosensor can detect anion using NH- fragment in the imidazole moiety of the structure. In this regard, UV-Vis absorption spectra were measured to investigate sensing properties of the probe toward different anions in DMSO. This chemosensor can detect both fluoride and cyanide ion with absorption change in intensity. In addition, pH sensing property was also investigated upon the addition of hydroxide ion. These properties are related to the deprotonation effect. The ICT system in this molecule was also observed by the computational approach using Material Studio 4.3 package.     

电子显微分析在表征纳米晶体化学组分中的应用

纳米材料的化学组分及含量影响其光、电、声、热、磁等物理性能,电子显微分析是表征纳米晶体化学组分的重要方法之一.本文综述了X-射线能谱(EDS)、X-射线波谱(WDS)、电子能量损失谱(EELS)和选区电子衍射(SAED)等现代电子显微分析技术在表征纳米晶体化学组分、形貌、尺寸和结构等方面的应用及其研究进展,并比较了这些分析方法存在的差异,提出了其应用中存在的不足及今后的研发方向.     

4- and 5-nitroindane

Mononitration of indane produces a mixture of 4- and 5- nitroindanes. Crystallization from mixtures occurs after distillation improves composition of a major component to above 80%. 4-Nitroindane: triclinic, space group (#2),a=7.332(4) Å,b=8.304(4) Å,c=8.358(4) Å, =61.43(4)°, =67.60(4)°, =70.15(4)°,V=405.4(4) ų,Z=2. Non-H-atoms are nearly planar, aliphatic H's are eclipsed. 5-Nitroindane: monoclinic, space groupP2₁/c (#14),a=10.946(8) Å,b=15.643(10) Å,c=9.415(6) Å, =92.34(5)°,V=1611(2) ų,Z=8. Non-H-atoms in the two molecules differ in torsion of the nitro group with respect to indane and fold of the nonbenzylic methylene group. Semiempirical calculations (PM3) suggest that distorsion from planarity may be associated with the two lowest energy vibrational modes. Uv, ir, ms, proton, and¹³C-nmr spectra are correlated with the solid state structures.     

6<Emphasis Type="Italic">S</Emphasis>,8α-Dihydroxy-14,15-Dihydrocarapin (Khayanone) from the Stem Bark of <Emphasis Type="Italic">Khaya Senegalensis</Emphasis> (Meliaceae): Isolation and its Crystal Structure

Khayanone was isolated from the stem bark of African mahogany, Khaya senegalensis (Meliaceae), and characterized as 6S,8α-dihydroxy-14,15-dihydrocarapin on the basis of spectral analysis and single crystal X-ray diffraction study. The compound crystallizes in the tetragonal space group P4 ₁ 2 ₁ 2 with unit cell parameters: a = 13.2315(19) Å, c = 29.118(6) Å, Z = 8. The crystal structure has been solved by direct methods and refined to R = 0.0375 for 4552 unique reflections. The six-membered rings A and B exist in boat conformations, rings C and D in chair conformations, and the furan ring is planar. The crystal structure is stabilized by O-H···O and C-H···O interactions. This is the first report about 6S configuration of mexicanolide revealed by X-ray diffraction analysis. The configuration of oxygenated C-6 in mexicanolide-group limonoids is discussed.     

Nuclear magnetic resonance: a powerful tool to study liquid crystals

Nuclear magnetic resonance (NMR) is a spectroscopic technique widely used to investigate materials and soft matter in particular. In this brief review, the main uses of NMR techniques to investigate different aspects of liquid crystals, such as the orientational and dynamic properties, the supramolecular structure and average molecular conformations, are described. In the second part of the paper, the case study of a ‘de Vries’ liquid crystal is reported and the main results obtained by combining different NMR techniques are discussed.     

X-ray analysis of sideroxol from <Emphasis Type="Italic">Sideritis leptoclada</Emphasis>

Sideroxol (1), a kaurane diterpene which has the ent-7α,18-dihydroxy-15β,16β-epoxykaurane structure (MW = 320.47, C₂₀H₃₂O₃) was obtained from the acetone extract of Sideritis leptoclada plant as well as from some other Sideritis species. It crystallizes in the orthorhombic space group P2₁, 2₁, 2₁ with a = 10.967(3), b = 24.555(5), c = 6.372(4) Å, Dc = 1.240 g cm⁻³, Z = 4, and refines to R = 0.065 for 721 independent reflections. The skeleton consists of three fused six-membered rings and a five-membered ring with fused epoxide. The six membered rings exhibited slightly distorted chair conformation. In addition to sideroxol, two kaurane and five kaurene diterpenes were isolated from the hexane and acetone extracts of the studied plant.     

New zeotype borophosphates with chiral tetrahedral topology: (H)0.5M1.25(H2O)1.5[BP2O8]·H2O (M = Co(II) and Mn(II))

Two new isostructural open‐framework zeotype transition metal borophosphate compounds, (H)_0.5M_1.25(H₂O)_1.5[BP₂O₈]·H₂O (M = Co(II) and Mn(II)) were synthesized by mild hydrothermal method. The structure of compounds were characterized by single‐crystal X‐ray diffraction which have ordered, alternating, vertex‐sharing BO₄, PO₄, and (MO₄)OM(H₂O)₂ groups with hexagonal, P 6₁ 2 2 (No 178) space group and unit cell parameters for Co a = 9.4960(6) Å, c = 15.6230(13) Å, for Mn a = 9.6547(12) Å, c = 15.791(3) Å, Z = 1 for both of them. TGA/DTA analysis, IR spectroscopy were used for characterization. Magnetic susceptibility measurements for both of the compound indicate strong antiferromagnetic interaction between metal centers. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)