沉积温度对Cu2O薄膜生长过程及光电性能的影响

以硫酸铜为铜源,采用一步化学浴沉积法制备出了晶粒尺寸可调的纳米晶Cu₂O薄膜。通过X射线衍射、扫描电镜和紫外可见分光光度法研究了沉积温度对薄膜晶体结构、成核密度、晶粒尺寸、薄膜厚度和光电性能的影响。结果表明,当在60~90℃范围内调节温度时,能够很好地控制晶粒尺寸、薄膜厚度,并将禁带宽度控制在33~51nm、392~556nm和2.47~2.61eV范围内;随着晶粒尺寸的减小,紫外可见光谱的吸收边有明显的蓝移。此外还对薄膜的生长过程,成核密度和颗粒尺寸变化的机理进行了讨论。     

结晶性和粒子尺寸对C60薄膜晶体管迁移率的影响

采用真空沉积方法在不同基片温度(30~190℃)和沉积压力(1×10~(-4)和1×10~(-1) Pa)下制得了C_(60)薄膜。研究了薄膜的结晶性和晶粒尺寸对迁移率的影响。采用X射线衍射和原子力显微镜表征了薄膜的结构和形貌,发现提高基片温度,薄膜的结晶性和晶粒尺寸均提高;提高沉积压力,薄膜的晶粒尺寸增大而结晶性不变。场效应测试结果表明,C_(60)薄膜的迁移率与其结晶性密切相关,高的结晶性有利于获得高迁移率;不同于平面有机半导体材料,对于球状C_(60)半导体材料,大的晶粒尺寸可能导致低迁移率。     

石墨烯氧化物薄膜电极的光电化学特性

采用浸渍-提拉法制备了一系列石墨烯氧化物(GO)薄膜,并通过X射线衍射(XRD),扫描电镜(SEM),傅里叶变换红外光谱,紫外-可见吸收光谱和光电化学测量等技术对样品进行了表征.在GO电极上观察到阴极光电流,且光电流密度受薄膜的厚度影响.GO薄膜电极厚度为27nm时,光电流密度为0.25μA·cm-2.此外,GO电极的光电响应还受紫外光照影响,随着紫外光照时间的延长,阴极光电流逐渐减小.该工作提供了简便的通过控制薄膜厚度或紫外光照时间来控制GO薄膜半导体光电化学性能的方法.     

基体表面性质对原位聚合沉积导电聚苯胺薄膜性能的影响

以水溶性高分子聚乙烯吡咯烷酮(PVP)为空间稳定剂,在经十八烷基三氯硅烷(OTS)改性的玻璃表面进行原位聚合,沉积得到导电聚苯胺(PANI)薄膜。采用表面界面张力仪、扫描电镜(SEM)、紫外可见光谱(UV-Vis)、红外光谱(FT-IR)、四探针电导率测试仪及光学显微镜对不同基体表面的接触角、PANI膜的形貌、厚度、结构、导电性及其在亲/憎水表面选择性沉积性能进行测定。结果表明:OTS对玻璃表面的改性促进了聚苯胺的沉积且提高了薄膜厚度,薄膜饱和厚度达到200 nm;缩短了溶液中苯胺分散聚合的诱导期,反应速率增大;与未改性玻璃表面沉积的薄膜相比,改性的玻璃表面得到的聚苯胺薄膜更加细密均匀,聚苯胺颗粒尺寸小,堆积紧密;薄膜的电导率达到7.5×10-3S/cm;OTS改性对基体表面的薄膜生长和溶液中的苯胺聚合具有催化作用。     

结晶性和粒子尺寸对C60薄膜晶体管迁移率的影响

采用真空沉积方法在不同基片温度（30~190℃）和沉积压力（1×10^-4和1×10^-1 Pa）下制得了C₆₀薄膜。研究了薄膜的结晶性和晶粒尺寸对迁移率的影响。采用X射线衍射和原子力显微镜表征了薄膜的结构和形貌,发现提高基片温度,薄膜的结晶性和粒子尺寸均提高;提高沉积压力,薄膜的晶粒尺寸增大而结晶性不变。场效应测试结果表明,C₆₀薄膜的迁移率与其结晶性密切相关,高的结晶性有利于获得高迁移率;不同于平面有机半导体材料,对于球状C₆₀半导体材料,大的晶粒尺寸可能导致低迁移率。     

退火温度对CdSe纳米薄膜的形成及光电性能影响

在室温下,采用循环伏安法在ITO上沉积CdSe纳米薄膜。利用X射线衍射仪(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(AFM)、X射线光电子能谱分析(XPS)、紫外-可见(UV-VIS)分光光度计以及电化学工作站对不同温度退火后的CdSe纳米薄膜的晶体结构、形貌、光学性能、光电化学性能进行表征和测试。结果表明,退火温度对CdSe纳米薄膜的形貌和性能起到关键性作用。薄膜表面平整、厚度均匀,且由呈纳米颗粒状的立方相CdSe构成;经退火后,CdSe纳米颗粒出现不同程度的长大现象,Se含量随退火温度的升高而减少。紫外-可见吸收光谱表明随着退火温度的升高,CdSe纳米薄膜对可见光的吸收发生红移,表明禁带宽度逐渐减小,表现出量子尺寸效应。通过光电流测试表明随着退火温度的升高,CdSe薄膜的光电响应效应显著提高。     

退火温度对CdSe纳米薄膜的形成及光电性能影响

在室温下,采用循环伏安法在ITO上沉积CdSe纳米薄膜。利用X射线衍射仪(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(AFM)、X射线光电子能谱分析(XPS)、紫外-可见(UV-VIS)分光光度计以及电化学工作站对不同温度退火后的CdSe纳米薄膜的晶体结构、形貌、光学性能、光电化学性能进行表征和测试。结果表明,退火温度对CdSe纳米薄膜的形貌和性能起到关键性作用。薄膜表面平整、厚度均匀,且由呈纳米颗粒状的立方相CdSe构成;经退火后,CdSe纳米颗粒出现不同程度的长大现象,Se含量随退火温度的升高而减少。紫外-可见吸收光谱表明随着退火温度的升高,CdSe纳米薄膜对可见光的吸收发生红移,表明禁带宽度逐渐减小,表现出量子尺寸效应。通过光电流测试表明随着退火温度的升高,CdSe薄膜的光电响应效应显著提高。     

苝染料杂化氧化锌薄膜的电沉积制备与表征

用含氯化锌(ZnCl2)和染料的二甲基亚砜溶液做电解液,可在ITO(氧化铟锡)导电玻璃上电化学沉积有机 无机杂化薄膜.薄膜的粒径尺寸约为300nm,杂化染料后的氧化锌(ZnO)薄膜的紫外可见吸收光谱相比纯ZnO薄膜明显宽泛而且偏向可见光部分.实验证明了染料敏化法提高ZnO薄膜光吸收能力的可行性.     

Ga对在AlN衬底上直接生长石墨烯的远程催化

通过镓(Ga)远程催化, 采用化学气相沉积(CVD)方法在氮化铝(AlN)衬底上直接生长石墨烯薄膜. 研究了生长温度、 催化剂距离对石墨烯生长及其光学性质和电学性质的影响规律. 结果表明, 在生长温度1070 ℃下可以制备厚度约为5层的石墨烯薄膜, Ga周围1.4 cm范围内可以得到厚度均匀的石墨烯薄膜. 通过透光率和方阻表征了石墨烯的光学和电学性质, 结果表明, 400~800 nm波长范围内石墨烯薄膜透光率可达90%以上, 方阻约为230 Ω/□. 第一性原理计算结果表明, 石墨烯仍保持金属性, AlN衬底对石墨烯有吸附掺杂作用, 可有效降低石墨烯的方阻, 改善石墨烯和衬底的电学接触.     

硫化镉纳米膜的生物还原-化学沉淀耦合制备及其性能表征

本文应用生物还原-化学沉淀耦合反应(CRBRCP-EDTA)制备出硫化镉纳米薄膜,并借助XRD和SEM对合成材料的物相、结构、形貌进行了表征。研究表明,以铝片为基底时CdS难以沉积,CdS纳米薄膜不能形成;以导电玻璃和单晶硅片为基底时CdS纳米薄膜方可生成。导电玻璃和单晶硅片薄膜都是双层结构,导电玻璃薄膜下层厚度大约40~50 nm,上层厚度大约450~500 nm,整体厚度大约500~550 nm;硅片薄膜的上下两层厚度基本相等,均为300 nm左右,而整体厚度达到600~650 nm。Cd²⁺浓度增加和分散剂PAM加入显著改善了导电玻璃薄膜质量,膜的致密性、均匀性和光催化活性都有所提高。     

Near infrared study of aqueous rare-earth ethylsulfates

The near infrared spectra of aqueous solutions of the ethylsulfates of La, Nd, Gd, Tb, Er, Yb, Lu, Y, and Na have been determined from about 0.2 mol-dm^–3 to nearly saturation. The extinction coefficients of water have been calculated taking into account the absorption of ethylslfate anions determined in separate experiments. Their values appeared to be nearly the same as that of pure water. The relative contents of free OH groups in 0.5 and 0.7M solutions have been estimated from the absorbances at 1160 nm. They were lower in solutions of the heavy rare-earth ethylsulfates (Tb, Er, Yb, Lu) than in equimolar solutions of the lighter ones (La, Nd), confirming our previous view that secondary hydration of the heavy trivalent rare-earth cations is distinctly stronger than that of the lighter ones. A comparison of the spectra of these aqueous ethylsulfates with those of perchlorates shows that the structure-breaking ability of the C₂H₅SO ₄ ^– ion is much smaller than that of perchlorate anion.     

Microstructures of Some Bi-W-Nb-O Phases

Microstructures of three Bi-W-Nb-O phases have been examined by using high-resolution transmission electron microscopy. Bi₁₇W₂Nb₃O₃₉ and Bi₁₇WNb₃O₃₆ have incommensurate superstructures derived from the defect fluorite-type δ-Bi₂O₃ and can be regarded as intermediate phases between the type II solid solutions in the Bi-Nb-O and Bi-W-O systems. Bi₈W₂Nb₂O₂₃ has a Bi₂WO₆-like subunit cell with a stepped superstructure. Formation mechanisms of various superstructures are discussed.     

Reactivity of Binary Mixtures of La(III) Oxide and Cu(II) Oxalate or Nitrate and Synthesis of La(III) Cuprate

Reactivity of mixtures of La(III) oxide and Cu(II) oxalate/nitrate in hydrated as well as anhydrous state was studied using TG, DTA and XRD. Cu(II) oxide formed in the endothermic decomposition of mixture containing hydrated Cu(II) nitrate and La(III) oxide could not form La₂CuO₄ while Cu(II) oxide formed in the exothermic decomposition of mixture containing hydrated/anhydrous Cu(II) oxalate and La(III) oxide reacts with La(III) oxide and develops the phases CuLaO₃ and La₂CuO₄. The maximum reactivity with respect to the formation of La₂CuO₄phase was observed in mixture containing anhydrous Cu(II) oxalate. This revised version was published online in July 2006 with corrections to the Cover Date.     

Preparation of ZrO2-TiO2-CeO2 and Its Application in the Selective Catalytic Reduction of NO with NH3

TiO₂,ZrO₂-TiO₂,andZrO₂-TiO₂-CeO₂ were prepared by co-precipitation method and characterized by X-ray diffraction (XRD), specific surface area measurements (BET), temperature programmed desorption (NH₃-TPD), oxygen storage capacity (OSC), and temperature programmed reduction (H₂-TPR). The results showed that ZrO₂-TiO₂-CeO₂ exhibited large number of surface strong acid, possessed some oxygen storage capacity, and strong redox property. The three materials were used as supports and the monolith catalysts were prepared with 1% (w) V₂O₅ and 9% (w)WO₃ for selective catalytic reduction (SCR) of NO with ammonia in the presence of excessive O₂, and the results of catalytic activity showed that the catalyst used ZrO₂-TiO₂-CeO₂ as support yielded nearly 100% NO conversion at 275 °C at a gas hourly space velocity (GHSV) of 10000 h⁻¹, and it had the best catalytic activity and showed great potential for practical application.     

电感耦合等离子体光谱法测定铜冶炼烟尘中锌

本实验介绍了电感耦合等离子体光谱法测定铜冶炼烟尘中锌含量的分析方法。针对样品碳,硅含量高的特点,有针对性的研究了样品的消解方法,确定采用盐酸、硝酸、氢氟酸、高氯酸对铜冶炼烟尘样品进行消解。同时进行了干扰试验,确定样品中高含量的铜,铅,砷等对样品测定结果没有影响。并对仪器的工作参数进行了优化。方法检出限为为0.011 mg/L,测定下限为0.019 mg/L,3个样品的相对标准偏差在0.54%~0.92%之间,加标回收率在96%~101.14%之间。该方法样品消解完全,流程短,操作简单,快速,测定准确度高,可以满足铜冶炼烟尘中锌含量的测定。     

Synthesis and characterization of gallium-based perovskitetype dense membrane with oxygen semipermeability

La0.15Sr0.85Ga0.3Fe0.7O3-δ(LSGFO) and La0.15Sr0.85Co0.3Fe0.7O3-δ(LSCFO) mixed oxygen-ion and electron conducting oxides were synthesized by using a combined EDTA and citrate complexing method, and the corresponding dense membranes were fabricated. The properties of the oxide powders and membranes were characterized with combined SEM, XRD, H2-TPR, O2-TPD techniques, mechanical strength and oxygen permeation measurement. The results showed that LSGFO had much higher thermochemical stability than LSCFO due to the higher valence stability of Ga3+. After the temperature-programmed reduction by 5% H2 in Ar from 20℃to 1020℃, the basic perovskite structure of LSGFO was successfully preserved. LSGFO also favors the oxygen vacancy formation better than LSCFO. Oxygen permeation measurement demonstrated that LSGFO had higher oxygen permeation flux than LSCFO, but they had similar activation energy for oxygen transportation, with a value of 110 and 117 kJ ?mol~(-1), respectively. The difference in oxygen permeation f     

Titania-supported mixed HPMoV polyoxometallates as precursors of hydrodesulfurization catalysts

HDS catalysts were prepared by loading H₃PMo₁₂O₄₀ or H₄PMo₁₁V₁O₄₀ polyoxometallates on TiO₂ (0.5 and 1.0 mmol (Mo+V)). Activity of the catalysts was tested in the HDS of thiophene. The activity of catalysts of low concentration was 2–3 times higher than the activity of those of high concentration. Temperature programmed reduction (TPR) and IR spectroscopy were used to determine the properties of the catalyst. TPR measurements proved that vanadium promotes and stabilizes HDS activity due to an increase in the Mo⁵⁺/Mo⁴⁺ ratio.     

α-Fe2O3掺杂对In2O3电导和气敏性能的影响

用化学共沉淀法制备了α Fe2O3掺杂的In2O3纳米晶微粉,研究了α Fe2O3掺杂对In2O3电导和气敏性能的影响. 结果表明, α Fe2O3和In2O3间可形成有限固溶体In2－xFexO3(0≤x≤0.40); Fe3＋对In2O3晶格中In3＋格位的部分取代,大大增强了阴阳离子间的结合力,导致材料中氧空位VO×数骤降、 自由电子的浓度变稀和电导下降. n(Fe3＋):n(In3＋)=5 :5的共沉淀粉于800 ℃下灼烧4 h所得的α Fe2O3掺杂In2O3传感器元件,对45 μmol•L－1 C2H5OH的灵敏度达54.0,为相同浓度干扰气体汽油的8倍多.     

电感耦合等离子体光谱法(ICP-AES)测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量

针对银精矿样品复杂,难消解的特点,研究了不同酸溶法和碱熔法对样品的消解情况,建立了硝酸,盐酸,氢氟酸,高氯酸消解银精矿的方法。根据元素灵敏度和抗干扰性,选定各元素的测定波长。通过酸溶样和碱熔样测定结果比对,验证了方法准确性。建立了四酸消解-电感耦合等离子体光谱法测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的方法,元素的线性相关系数均在0.9999以上。通过共存元素干扰实验,确定了银精矿中高含量元素(铜、铅、锌、铁、锑、铋等)对测定元素结果没有影响。方法检出限：Cu 0.0063 mg/L, Pb 0.0159 mg/L ,Zn 0.0090 mg/L,As 0.0192 mg/L, Cd 0.0093 mg/L ,Ca 0.0084 mg/L, Mg 0.0075 mg/L, Mn 0.0081 mg/L。测定下限：Cu 0.0105mg/L,Pb 0.0265 mg/L, Zn 0.0150 mg/L, As 0.0320 mg/L, Cd 0.0155 mg/L, Ca 0.0140 mg/L, Mg 0.0125 mg/L,Mn 0.0135 mg/L。3个样品的相对标准偏差在0.87%~3.56%之间,加标回收率在95.00%~103.56%之间。方法流程短,操作简单,快速,灵敏度和再现性高,结果准确可靠,可以满足银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的测定。     

Li_(1.3)Ti_(1.7)Al_(0.3)(PO_4)_3,Na_(1.3)Ti_(1.7)Al_(0.3)(PO_4)_3的离子交换研究

研究了在不同温度下的NaNO3和AgNO3水溶液中Li1.3Ti1.7Al0.3(PO4)3和Na1.3Ti1.7Al0.3(PO4)3离子交换行为.实验表明Li1.3Ti1.7Al0.3(PO4)3和Na1.3Ti1.7Al0.3(PO4)3均显示出了高选择性与Na+和Ag+进行离子交换的特征,且对Ag+的选择性高于Na+.升高温度可显著提高Ag/Li和Ag/Na的交换反应速度.