射频磁控溅射生长ZnO薄膜及性能研究

采用射频磁控溅射技术在玻璃衬底生长ZnO及ZnO∶ Al薄膜,通过改变氩氧比、衬底温度和溅射功率获得样品.用X射线衍射仪、紫外-可见分光光度计、扫描电子显微镜进行表征.结果发现:室温下40W的溅射功率1h的溅射时间,改变氩氧比获得样品.XRD图谱中无明显衍射峰出现;紫外可见光分光光度计测试结果显示400nm波长以下,透光率在90;以上.说明薄膜生长呈无定形.衬底温度高于200℃样品,XRD有明显(002)衍射峰出现,在400～ 800 nm波长范围,透光率在88;以上,衬底温度300℃时,XRD衍射峰半高宽最小,晶粒尺寸大.TEM显示:衬底300℃晶粒尺寸最大,晶体发育好.在200℃掺铝ZnO薄膜,(002)峰不明显,有(101)峰出现.     

衬底温度对磁控溅射法制备掺Ta氧化锌薄膜性能的影响

采用射频磁控溅射法,在不同的衬底温度下制备了钽(Ta)掺杂的氧化锌(ZnO)薄膜,采用X射线能谱(EDS)、X射线衍射(XRD)、扫描电镜(SEM)、紫外-可见分光光度计和光致发光(PL)光谱研究了衬底温度对制备的Ta掺杂ZnO薄膜的组分、微观结构、形貌和光学特性的影响.EDS的检测结果表明,Ta元素成功掺入到了ZnO薄膜;XRD图谱表明,掺入的Ta杂质是替代式杂质,没有破坏ZnO的六方晶格结构,随着衬底温度的升高,(002)衍射峰的强度先增大后降低,在400℃时达到最大;SEM测试表明当衬底温度较高时(400℃和500℃),Ta掺杂ZnO薄膜的晶粒明显变大;紫外-可见透过光谱显示,在可见光范围,Ta掺杂ZnO薄膜的平均透光率均高于80;,衬底不加热时制备的Ta掺杂ZnO的透光率最高;制备的Ta掺杂ZnO薄膜的禁带宽度范围为3.34~3.37eV,衬底温度为500℃时制备的Ta掺杂ZnO薄膜的禁带宽度最小,为3.34eV.PL光谱表明衬底温度为500℃时制备的Ta掺杂ZnO薄膜中缺陷较多,这也是造成薄膜禁带宽度变小的原因.     

衬底温度对PLD方法制备的ZnO薄膜的光学和电学特性的影响

利用脉冲激光沉积法(PLD)在c面蓝宝石衬底上制备了ZnO薄膜并对其进行了X射线衍射(XRD)、反射式高能电子衍射(RHEED)、光致发光(PL)谱和霍尔(Hall)测试.RHEED和XRD分析表明,温度在350℃至550℃之间时,ZnO薄膜的结晶质量随着衬底温度的升高而提高,当衬底温度进一步升高后,ZnO薄膜的结晶质量开始下降.四个样品中,衬底温度为550℃的样品具有最清晰的规则点状RHEED图像和半高宽最窄的(0002)衍射峰.PL谱和Hall测量的结果表明,衬底温度为550℃的样品还具有最好的发光性质和最大的霍尔迁移率.     

在钛酸锶衬底上外延生长ZnO薄膜及其性能研究

用脉冲激光淀积法(PLD)在(111)面SrTiO3衬底上外延生长ZnO单晶薄膜.样品分别在衬底温度为350℃、500℃、600℃下外延生长.X射线衍射(XRD)的结果表明,所得的ZnO单晶薄膜结晶性能好,只出现(002)和(004)两个衍射峰,(002)峰的半高宽度(FWHM)为0.23°.在荧光光谱中我们只观察到来源于带边激子跃迁的强UV发射,并且随着生长温度的升高,紫外峰的强度逐渐增强.样品的SEM图像表明所得ZnO薄膜表面平整,晶粒均匀.衬底温度为600℃时,所得到的ZnO薄膜结构完整,晶粒尺寸最大,均匀;而且紫外发射最强.     

退火温度对6H-SiC衬底上ZnO薄膜发光性质的影响

采用溶胶-凝胶方法,在6H-SiC衬底上制备ZnO薄膜.X射线衍射结果表明薄膜是c轴取向的,具有六方纤锌矿多晶结构.研究了退火温度对ZnO薄膜发光特性的影响.发现在650℃退火温度下,观察到近带边紫外发射和可见光发射并且紫外发光强度大于可见光发射.随着退火温度的提高,紫外峰强度减弱直至消失,而绿光发射强度先增加而后降低.对退火温度引起ZnO薄膜发光性质改变的机制进行了探讨.     

(111)择优取向ZnS薄膜的制备及特性研究

采用激光分子束外延技术在Al2O3衬底上成功外延生长了ZnS薄膜.用X射线衍射、扫描电子显微镜和光致发光谱表征了衬底温度对薄膜结构、形貌和光学特性的影响.结果表明所生长的ZnS薄膜为闪锌矿,具有(111)择优长向,随衬底温度的升高,X射线衍射峰的半高宽先减小后增大,在衬底温度为300℃时,半高宽最窄.薄膜结构致密,表面不平整度随衬底温度的升高而增大.薄膜的带隙随衬底温度的升高出现蓝移,可见光区域透射率最高达到98;,在360 nm激发波长下,观测到402 nm和468 nm两个发光带,衬底温度为300℃时,发光最强.     

MOCVD法在(220)CaF2衬底上生长ZnO薄膜及其性能研究

采用金属有机化学汽相沉积(MOCVD)法在(220)CaF2衬底上外延生长ZnO薄膜.利用X射线衍射(XRD)、紫外-可见光谱和光致发光谱(PL)对ZnO薄膜的结构和光学性能进行了分析.XRD结果表明,所制备的ZnO薄膜结晶性能良好,具有高度的(002)的择优取向,002衍射峰的半高宽(FMHM)为0.115°.所制备的ZnO薄膜透明,透过率超过85;.在常温的(He-Cd激光器)PL谱中,只有378.5 nm的带边发射.用同步辐射光源测试的真空紫外光谱中,在低温20K时,出现218 nm、368 nm、418 nm、554 nm发光峰,其中368 nm峰强度随着温度的升高强度逐渐下降,到常温时几乎消失.     

超声喷雾热分解法制备ZnO薄膜及衬底温度对其性能的影响

以醋酸锌水溶液为前驱体溶液,采用超声喷雾热分解法在玻璃衬底上制备得到了温度在350℃到450℃范围内的ZnO薄膜.用X射线衍射(XRD)、扫描电镜(SEM)及紫外-可见分光光度计分析了ZnO薄膜的晶体结构、微观形貌及其光学性质,重点探究了衬底温度对ZnO薄膜生长过程及微观结构的影响.分析表明:制备的ZnO薄膜为六角铅锌矿结构,衬底温度对薄膜的质量有着重要的影响;所得薄膜在400℃时结晶性能好,沿c轴择优取向生长,具有优良的均匀性和致密性;所制备的薄膜在可见光区透过率高达86;以上,在紫外光区吸收强烈.     

退火对Si(111)衬底上ZnO薄膜的结构和发光特性的影响

采用磁控溅射法在硅(111)衬底上制备了C轴高度取向的ZnO薄膜,并研究了退火温度和氧气气氛对ZnO薄膜晶体质量、晶粒度大小和光致发光谱的影响.X射线衍射表明,所有薄膜均为高度C轴择优取向,当退火温度低于900℃时,随着退火温度的升高,薄膜的取向性和结晶度都明显提高.室温下对ZnO薄膜进行了光谱分析,退火后的样品均可观测到明显的紫光发射.在一定的退火温度范围内,还可以观测到明显的紫外双峰.空气中退火的样品,当退火温度达到或高于600℃还可观测到绿光发射.实验结果表明,发光峰强度随退火温度和氧气气氛不同而不同,通过改变退火时的温度和氧气气氛可以改变ZnO薄膜的微结构和发光性质.     

退火温度对Li:ZnO薄膜紫外发射性能影响

利用溶胶-凝胶法在Si衬底上制备不同退火温度的Li∶ZnO薄膜。借助X射线衍射(XRD)、X射线光电子谱(XPS)、扫描电镜(SEM)和光致发光(PL)谱研究样品结晶质量、成分、表面形貌和发光特性。结果表明:所有样品均高度c轴择优取向生长;随退火温度升高,样品结晶性变好,紫外发射增强。LiOH在退火温度超过700℃分解,使Li、H进入到ZnO晶格,在ZnO薄膜中形成LiZn-H复合缺陷,这种复合缺陷使H被困在ZnO薄膜中,形成H施主,显著提高ZnO薄膜紫外发光强度,抑制ZnO薄膜绿光发射。     

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。     

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.     

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。     

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.     

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.