以SBA-16薄膜/ITO为基底电沉积生长“花状”CdS纳米晶体

在酸性条件下,以导电玻璃(ITO)为基底合成sBA.16分子筛膜.所制备的SBA-16薄膜孔径均匀,具有体心立方结构(属于Im3m空间群).在由CdCl2和Na2S2O3组成的电解液中,调节pH值为2～3.利用直流恒电位电沉积法,调节电位为-0.7 V,沉积时间为50 min,在SBA-16膜/ITO电极表面电沉积生长出"花状"CdS纳米晶体,利用SEM、TEM等技术研究了CdS纳米晶体形貌和结构,同时进行了荧光光谱测试.结果表明,电沉积合成的CdS生长在电极表面而不是生长在介孔孔道中.并能够产生荧光谱峰.     

电化学沉积制备半导体CuInSe2薄膜

本文报道恒电位法在pH为1.35的Cu₂SO₄、SeO₂、In₂(SO₄)₃溶液中,在Ti电极上电化学沉积制备CuInSe₂纳米薄膜.研究络合剂柠檬酸和酒石酸对制备CuInSe₂纳米薄膜的影响.扫描电子显微镜(SEM)结果表明,加入络合剂后,电化学沉积的薄膜表面颗粒分布更均匀、致密.X射线衍射(XRD)分析显示,制备的CuInSe₂薄膜是黄铜矿和闪锌矿相的混和物,添加柠檬酸和酒石酸后,衍射峰增强,晶形变好.制备的薄膜颗粒尺寸大小在250nm左右,造成粒度增大的原因是由于颗粒的团聚作用.     

液相沉积法制备ZnO/CdS复合纳米棒阵列薄膜及其光电性质

采用两步化学溶液沉积法在氧化铟锡(ITO)导电玻璃衬底上制备了ZnO/CdS复合纳米棒阵列薄膜.利用X射线衍射(XRD)仪、扫描电子显微镜(SEM)、紫外-可见(UV-Vis)吸收分光光度计、荧光(PL)光谱仪及表面光电压谱(SPS)研究了不同CdS沉积时间对复合薄膜的晶体结构、形貌、光电性质的影响.研究结果表明:ZnO纳米棒阵列表面包覆CdS纳米颗粒后,其吸收光谱可拓展到可见光区;与吸收光谱相对应在可见光区出现新的光电压谱响应区,这一现象证实,通过与CdS复合可显著提高ZnO纳米棒阵列在可见光区的光电转换性能;随着CdS纳米颗粒沉积时间的延长,复合纳米棒阵列薄膜在大于383nm波长区域的光电压强度逐渐减弱,而在小于383nm波长区域的光电压强度逐渐增强.用两种不同的电荷产生和分离机制对这一截然相反的光响应过程进行了详细的讨论和解释.     

非晶纳米高熵合金薄膜Nd-Fe-Co-Ni-Mn的电化学制备及磁学性能

通过电沉积方法在室温下制备了具有纳米结构组织的Nd-Fe-Co-Ni-Mn高熵合金磁性薄膜。 通过改变电沉积参数,如沉积电位、沉积时间,可控制薄膜的纳米结构及表面形貌。 扫描电子显微镜观察结果表明,在Ti基体上,-2.2 V下沉积5 min可制备出大小在200 nm左右的均匀分布的球形颗粒薄膜,延长沉积时间会使薄膜变得更加致密,而沉积电位的负移会导致纳米片的出现。 能谱结果表明5种元素发生了共沉积,结构分析表明该薄膜是无定形态的。 稀土元素Nd与过渡金属发生共沉积,可能是由于过渡金属离子与二甲基亚砜形成多核配位化合物而使得过渡金属离子沉积电位负移所致。 Nd-Fe-Co-Ni-Mn高熵合金薄膜在室温下具有良好的软磁性能。     

ITO/TiO2表面电沉积CdS纳米粒子及其薄膜的光电性能

采用阴极恒电位沉积方法, 在TiO2表面沉积制备出CdS纳米粒子. XRD和SEM测试结果表明, CdS粒子的结构以六方晶相为主, 粒径分布均匀, 表面形貌呈菜花状. 通过调节沉积电位和沉积时间等因素在一定程度上可以控制CdS纳米粒子的生长. 随着沉积电位变负, CdS粒子的粒径逐渐减小. 沉积时间越短, 粒子粒径越小. 紫外-可见吸收光谱测试结果表明, 不同条件下制备出来的CdS粒子表现出一定的量子尺寸效应. 此外, 沉积条件也会影响ITO/TiO2/CdS复合半导体薄膜的光电性能.     

壳聚糖-CdS复合膜制备及其对吡啶的传感特性

利用壳聚糖（CS）易于成膜的特点，模拟生物矿化，在有机物调制下通过异相成核生长制备了CS/CdS纳米颗粒复合膜.研究了成膜条件对膜的水热稳定性和发光性能的影响，以及CS/CdS纳米颗粒复合膜对水体中吡啶的响应特性.扫描电镜分析表明CS/CdS纳米颗粒复合膜均匀性好， CdS以物理掺杂方式均匀分布于CS薄膜中， CdS颗粒尺寸在70 nm左右.但薄膜荧光光谱位置和形状表明实际发光的CdS簇集体直径小于20 nm.由此推测电镜观察到的CdS颗粒可能是由许多CdS小颗粒聚集而成，小颗粒之间因有机物的存在而相互隔离. CS/CdS纳米颗粒复合膜的荧光发射对水体中吡啶的存在十分敏感，微量吡啶的存在会引起薄膜荧光发射急剧增强.除铜和碘离子外，水体系中其他常见离子对薄膜荧光发射没有显著影响，预期CS/CdS纳米颗粒复合薄膜有可能发展成为一种重要的水体系吡啶测定专用传感薄膜材料.     

TiO2薄膜的Ag改性及光催化活性

 用光化学沉积法对纳米TiO2薄膜进行了Ag改性,用漫反射紫外-可见光谱、扫描电子显微镜和X射线光电子能谱分析了Ag-TiO2薄膜的光谱特征、表面形貌和表面组成. 以苯酚为模拟污染物,在不同波长光源及有氧和无氧条件下考察了Ag-TiO2薄膜的光催化活性. 结果表明,当银沉积量大于 0.0150 mg/cm2时, Ag-TiO2薄膜对紫外光的吸收发生了明显的蓝移,同时在346 nm附近出现了小的吸收峰且该峰随着银沉积量的增加逐渐向长波方向移动. 沉积在TiO2薄膜表面的银颗粒大小不均匀,主要以单质银的形式存在,也生成了部分Ag2O; 相对于TiO2薄膜, Ag-TiO2薄膜表面吸附氧的含量明显增大. Ag-TiO2薄膜的光吸收特性对其催化活性影响较大. 在低压汞灯及有氧参与的条件下,银沉积量为0.0523 mg/cm2的Ag-TiO2薄膜的催化活性最高, 其反应速率常数是TiO2薄膜的1.16倍. Ag+更易沉积在较大n值的Ag簇上,其颗粒大小不可能完全均匀. Ag-TiO2薄膜的光吸收特性、 Ag簇的大小以及Ag对O2的吸附作用是决定Ag-TiO2薄膜催化活性的主要因素.     

硫化镉纳米线的电沉积制备及表征

以不同孔径的多孔阳极氧化铝为模板,采用直流电沉积的方法,在含CdCl2和S的DMSO溶液中制备出了CdS纳米线．SEM、TEM表征的结果表明,在不同孔径的多孔阳极氧化铝模板中,通过沉积时间等条件的控制,制得直径不同、长度可达5μm的平行结构、均匀而连续的CdS纳米线阵列．电子衍射和能谱结果显示所得的纳米线属于六方晶系CdS,线中Cd和S原子比接近1：1．     

电沉积WO_3薄膜及其光电性能的表征

本文采用电化学法制备了均匀、附着力强的WO3薄膜,研究了不同沉积电位和不同的沉积时间对薄膜的光电性能影响,并使用了XRD,UV-vis,M-S,光电流光谱(IPCE)等分析表征手段对薄膜进行了表征。实验结果表明,所制得的WO3薄膜为单斜晶系,退火后沿(200)晶面择优生长;对比所有沉积电位,-0.45 V沉积电位(vs.SCE)所获得的WO3薄膜均匀致密,薄膜的带边在460 nm(≈2.7 eV),其光电转换性能最好;在实验范围内薄膜越厚,其光电转换性能越好。     

电沉积法制备介孔TiO_2/CdS薄膜光电极

采用阴极恒电位沉积法,在介孔TiO2薄膜上制备了介孔TiO2/CdS薄膜光电极,用XRD,SEM,Raman,SPS和UV-Vis等多种手段对薄膜电极进行了表征.结果表明,CdS成功沉积到介孔TiO2的表面和孔道内,形成了异质结结构.通过光电流作用谱考察了该复合体薄膜电极的光电性能,结果表明,与单纯的介孔TiO2薄膜相比,其光电转换效率显著提高,这是由于CdS具有吸收可见光的特性以及CdS与介孔TiO2形成异质结从而使得光生载流子更容易分离的结果.     

Pulsed Laser Deposition ZnS Buffer Layers for CIGS Solar Cells

Polycrystalline ZnS films were prepared by pulsed laser deposition （PLD） on quartz glass substrates under different growth conditions at different substrate temperatures of 20, 200, 400, and 600 ℃, which is a suitable alternative to chemical bath deposited （CBD） CdS as a buffer layer in Cu（In,Ga）Se2 （CIGS） solar cells. X-ray diffraction studies indicate the films are polycrystalline with zinc-blende structure and they exhibit preferential orientation along the cubic phase β-ZnS （111） direction, which conflicts with the conclusion of wurtzite structure by Murali that the ZnS films deposited by pulse plating technique was polycrystalline with wurtzite structure. The Raman spectra of grown films show Al mode at approximately 350 cm^-1, generally observed in the cubic phase β-ZnS compounds. The planar and the cross-sectional morphology were observed by scanning electron microscopic. The dense, smooth, uniform grains are formed on the quartz glass substrates through PLD technique. The grain size of ZnS deposited by PLD is much smaller than that of CdS by conventional CBD method, which is analyzed as the main reason of detrimental cell performance. The composition of the ZnS films was also measured by X-ray fluorescence. The typical ZnS films obtained in this work are near stoichiometric and only a small amount of S-rich. The energy band gaps at different temperatures were obtained by absorption spectroscopy measurement, which increases from 3.2 eV to 3.7 eV with the increasing of the deposition temperature. ZnS has a wider energy band gap than CdS （2.4 eV）, which can enhance the blue response of the photovoltaic cells. These results show the high-quality of these substitute buffer layer materials are prepared through an all-dry technology, which can be used in the manufacture of CIGS thin film solar cells.     

Preparation and Magnetic Properties of Submicron CrO2 Thin Film on Poly-crystal TiO2 Film

The submicron chromium dioxide(CrO₂) thin film was fabricated on a poly-crystal titania(TiO₂) film using Si wafers as substrates by atmospheric pressure chemical vapor deposition(CVD) method. X-Ray diffraction patterns show that the CrO₂ films were pure rutile structure. Scanning electron microscopy(SEM) images indicate that the CrO₂ films consisted of submicron grains with a grain size of 250―750 nm. The magnetic researches reveal that the magnetic easy axis is parallel to the films, and at room temperature, the CrO₂ films show linear magnetoresistance.     

CdS Thin Films Deposited by CBD Method on Glass

CdS thin films were prepared by chemical-bath-deposited method and the effect of tempera-ture and time on the properties of CdS thin films was studied. Independent of the deposited temperature, the growth was mainly controlled by the ion-by-ion growth mechanism at the beginning of the film deposition, then the cluster-by-cluster mechanism came to be domi-nant. The growth rate increased faster with the increasing of temperature until the thickness reached the limitation, then thickness instead become thinner. The scanning electron micro-scope results revealed that the morphology of the CdS film changed from pinholes to rough,inhomogeneous surface with increasing deposition time and deposition temperature. The X-ray diffraction results showed the film structure was a mixture of two phases: hexagonal and cubic, and it was very important to controll deposition time to the film's crystal phase. All films in depth of approximate 100 nm existed above 65% transmittance, the absorption edge became 〝red-shift〞 with temperature rising. At 60 and 70 oC, with 20 min deposited-time, the energy band gap was more than 2.42 eV and decreased with time, while at 80 and 90 oC, the energy band gap was less than 2.42 eV and increased little when the time changed from 10 min to 15 min at 80 oC.     

Creation of high-refractive-index amorphous titanium oxide thin films from low-fractal-dimension polymeric precursors synthesized by a sol-gel technique with a hydrazine monohydrochloride catalyst

Amorphous titanium dioxide (TiO(2)) thin films exhibiting high refractive indices (n ≈ 2.1) and high transparency were fabricated by spin-coating titanium oxide liquid precursors having a weakly branched polymeric structure. The precursor solution was prepared from titanium tetra-n-butoxide (TTBO) via the catalytic sol-gel process with hydrazine monohydrochloride used as a salt catalyst, which serves as a conjugate acid-base pair catalyst. Our unique catalytic sol-gel technique accelerated the overall polycondensation reaction of partially hydrolyzed alkoxides, which facilitated the formation of liner polymer-like titanium oxide aggregates having a low fractal dimension of ca. (5)/(3), known as a characteristic of the so-called "expanded polymer chain". Such linear polymeric features are essential to the production of highly dense amorphous TiO(2) thin films; mutual interpenetration of the linear polymeric aggregates avoided the creation of void space that is often generated by the densification of high-fractal-dimension (particle-like) aggregates produced in a conventional sol-gel process. The mesh size of the titanium oxide polymers can be tuned either by water concentration or the reaction time, and the smaller mesh size in the liquid precursor led to a higher n value of the solid thin film, thanks to its higher local electron density. The reaction that required no addition of organic ligand to stabilize titanium alkoxides was advantageous to overcoming issues from organic residues such as coloration. The dense amorphous film structure suppressed light scattering loss owing to its extremely smooth surface and the absence of inhomogeneous grains or particles. Furthermore, the fabrication can be accomplished at a low heating temperature of <80 °C. Indeed, we successfully obtained a transparent film with a high refractive index of n = 2.064 (at λ = 633 nm) on a low-heat-resistance plastic, poly(methyl methacrylate), at 60 °C. The result offers an efficient route to high-refractive-index amorphous TiO(2) films as well as base materials for a wider range of applications.     

一种在室温合成具有宽带隙CdS的简单方法

采用简单的磁控溅射方法, 在室温合成了CdS多晶薄膜. 在溅射CdS多晶薄膜过程中, 分别在Ar 气中通入0%、0.88%、1.78%、2.58%和3.40% (体积分数, φ)的O₂, 得到不同O含量的CdS多晶薄膜. 通过X射线衍射仪、拉曼光谱仪、扫描电子显微镜、X射线光电子能谱仪、紫外-可见光谱仪对得到的CdS多晶薄膜进行表征.分析结果表明: O的掺入能得到结合更加致密, 晶粒尺寸更小的CdS多晶薄膜; 与溅射气体中没有O₂时制备的CdS多晶薄膜的光学带隙(2.48 eV)相比, 当溅射气体中O₂的含量为0.88%和1.78% (φ)时, 制备得到的CdS多晶薄膜具有更大的光学带隙, 分别为2.60和2.65 eV; 而当溅射气体中O₂的含量为2.58%和3.40% (φ)时, 得到的CdS光学带隙分别为2.50 和2.49 eV, 与没有掺杂O的CdS的光学带隙(2.48 eV)相当; 当溅射气体中O₂的含量为0.88% (φ)时, 制备的CdS多晶薄膜具有最好的结晶质量. 通过磁控溅射方法, 在溅射气体中O₂含量为0.88% (φ)条件下制备的CdS多晶薄膜表面沉积了CdTe 多晶薄膜并在CdCl₂气氛中进行了高温退火处理, 对退火前后的CdTe多晶薄膜进行了表征. 表征结果显示: CdS中掺入O能得到结合更紧密、退火后晶粒尺寸更大的CdTe多晶薄膜. 通过磁控溅射方法, 在CdS制备过程中于Ar 中掺入O₂, 在室温就能得到具有更大光学带隙的CdS多晶薄膜, 该方法是一种简单和有效的方法, 非常适用于大规模工业化生产.     

Plan-view preparation of TEM specimens from thin films using adhesive tape

A simple plan-view sample preparation technique for transmission electron microscopy (TEM) specimens is proposed for thin films by tearing-off the film with adhesive tape. The demand for very thin samples is highest for nanostructured materials where the structure of 2-5 nm sized features (grains) needs to be resolved; therefore, overlapping of nanometer-sized features should be avoided. The method provides thin areas at the fracture edges of plan-view specimens with thickness in the range of the grain size in the film allowing for artifact free high-resolution TEM imaging. Nanostructured materials typically fracture between the grains providing areas with the thickness of the grain size. Besides the swiftness of the method, the samples are free of surface amorphization artifacts, which can occur in ion beam milling up to 1 nm depth even at low energy ion bombardment. The thin film tear-off technique is demonstrated on a CuMn alloy thin film with grain size of 2 nm.     

CdS量子点敏化ZnO纳米棒阵列电极的制备和光电化学性能

采用连续式离子层吸附与反应法制备了CdS量子点敏化的ZnO纳米棒电极.应用扫描电子显微镜(SEM)、X射线衍射(XRD)和透射电子显微镜(TEM)对CdS量子点/ZnO纳米棒电极的形貌、晶型和颗粒尺寸进行了分析和表征;采用光电流-电位曲线和光电流谱研究了不同CdS循环沉积次数及不同沉积浓度对复合电极的光电性能影响.结果表明,前驱体浓度都为0.1mol·L-1且沉积15次敏化后的ZnO纳米棒阵列电极光电性能最好.与单纯的ZnO纳米棒阵列电极和单纯的CdS量子点电极相比,其光电转换效率显著提高,单色光光子-电流转换效率(IPCE)在380nm处达到76%.这是因为CdS量子点可以拓宽光的吸收到可见光区,并且在所形成的界面上光生载流子更容易分离.荧光光谱实验进一步说明了光电增强的原因是,两者间形成的界面中表面态大大减少,有利于减少光生电子和空穴的复合.     

Atomically flat gold on elastomeric substrate

We present a procedure to fabricate extremely smooth Au films supported on thin elastomeric (PDMS) substrates. Minimum rms roughness and largest grain size are obtained using Si wafers, coated with native oxide and release layers, as templates for the growth of thermally evaporated Au films. The wafers are held at a temperature of 300 degrees C during deposition. The Au films, up to 200 nm thick, are then transferred onto poly(dimethylsiloxane) substrates which have been previously surface-functionalized with a (3-mercaptopropyl)trimethoxysilane adhesion layer. The resulting Au films have been found by AFM to be extremely smooth with rms-roughness 2.5-4 angstroms and to exhibit a crystalline morphology with flat grains >500 nm in size. Thinner films, down to 20 nm, are grown at lower temperature and are comparably smooth, but with a loss in crystalline morphology. We compare the results of this optimized procedure with other gold films grown on mica sheets as templates and to those produced using Ti-O-Si interfacial chemistry.     

Elaboration and characterization of La2NiO4+δ powders and thin films via a modified sol–gel process

Polycrystalline thin films of La₂NiO_4+δ have been synthesized on yttria stabilized zirconia (YSZ) substrates by dip-coating using a polymeric sol. Crack-free films were obtained after sintering in air at temperatures ranging from 800°C to 1000°C. The microstructure, characterized by SEM, shows the formation of dense polycrystalline films with smooth surface and mean grains size of 140 nm, for films sintered at 1000°C. A correlation between grains size and non-stoichiometry in powders have been made in our processes. The thickness, evaluated for rugosimetry measurements, is thin (80 nm) and is a function of the viscosity of the sol. The higher the thickness, the higher the viscosity. As the non-stoichiometry level is controlled by the oxygen partial pressure, an evolution of non-stoichiometry in thin film has proposed. Then, it is possible by modifying synthesis and processing parameters to prepare thin films with a controlled microstructure (thickness, porosity and non-stoichiometry).     

Growth control of homogeneous pulsed electrodeposited Co thin films on n-doped Si(1 1 1) substrates

Cobalt thin films were deposited by pulsed electrodeposition on n-doped silicon substrates. We show that the morphology and the magnetic properties of the samples can be controlled by a careful choice of the deposition conditions. Atomic force microscopy measurements reveal a granular growth with grain size and homogeneity strongly dependent on the total deposition time and pulse frequency of the applied signal. Magnetic force microscopy and magnetization measurements indicate the formation of magnetically correlated grain systems with a maximum magnetic correlation and homogeneity for samples with grain diameters of about 40 nm.