非晶硅薄膜制备及其晶化特性研究

用磁控溅射法在K9玻璃上沉积了非晶硅(a-Si)膜和a-Si/Al膜,并将其在流动的N2气氛下进行退火.对退火前后的样品进行Raman光谱、XRD和SEM表征和分析.Raman光谱表明随着退火温度的升高,a-Si膜的散射峰出现了明显的蓝移,但XRD结果表明薄膜仍为非晶态;而a-Si/Al膜在温度很低时就已经开始晶化.     

低温水热法制备高催化效率钒酸铋可见光催化剂

采用低温水热合成法,通过控制反应体系pH值实现了对晶体形貌的调控,制备了高催化效率的单斜相钒酸铋催化剂.对样品进行了X射线衍射、紫外可见漫反射吸收光谱、扫描电镜和比表面积分析,并以罗丹明B的降解考察了样品的光催化活性.结果表明,反应体系pH值影响钒酸铋的形貌和光催化性能,pH值为7条件下制备得到的BiVO4样品对罗丹明B的光催化降解率最大,光催化反应lh对罗丹明B的降解率为93.56;.H2O2作为电子捕获剂,与电子反应形成羟基自由基,抑制电子和空穴对的复合,H2O2协同催化显著提高了光催化效率.     

常规退火与光退火固相晶化的对比

为研究传统炉子退火与光退火固相晶化的不同特点,用石英玻璃作衬底,在室温、350℃和450℃下用PECVD法直接沉积非晶硅(a-Si:H)薄膜,把沉积的样品分别在850℃下用传统炉子退火3h、用光快速热处理(RTP)5min,然后用Raman、XRD和SEM分析对比,发现传统炉子退火后的晶粒分布不均匀,光退火后的晶粒分布均匀.XRD分析发现两种方法晶粒尺寸均为30nm左右.     

利用快速热退火法制备多晶硅薄膜

为了制备优质的多晶硅薄膜,该论文研究了非晶硅薄膜的快速热退火(RTA)技术.先利用PECVD设备沉积非晶硅薄膜,然后把其放入快速热退火炉中进行退火.退火前后的薄膜利用X射线衍射(XRD)仪、Raman光谱仪及扫描电子显微镜(SEM)测试其晶体结构及表面形貌,利用电导率测试设备测试其暗电导率.研究表明退火温度、退火时间以及沉积时的衬底温度对非晶硅薄膜的晶化都有很大的影响.     

TiO2-Pt-CoPi三元复合物的制备、表征和光催化性能研究

以钛酸正丁酯TBT为原料,采用水热法制备了TiO2纳米片,并用光沉积法将Pt纳米颗粒和CoPi催化剂分步沉积在TiO2纳米片上,制备TiO2-Pt-CoPi三元复合物.利用X射线衍射(XRD)、扫描电镜(SEM)等对样品进行了表征,测试了三元复合物的光催化活性.实验结果表明,通过控制光沉积时间、顺序等因素对复合光催化剂的光催化性能进行优化,大大提升了其完全光解水的光催化活性.     

CuAlSe2光伏吸收层薄膜的制备

用同族元素Al和Fe取代CulnGaSe2薄膜中的In和Ga元素.采用粉末冶金工艺制备CuAlSe2和CuAlSe2∶Fe光伏吸收层薄膜.依次对薄膜样品进行了表面形貌、化学成分、薄膜厚度、晶体结构和光学特性测试分析.结果表明,退火温度为450℃、500℃、550℃时薄膜的生长特性较好,薄膜较为致密,结晶度较高.薄膜主要为黄铜矿结构,并沿(112)晶相择优生长.CuAlSe2薄膜和CuAlSe2∶Fe薄膜样品的光学吸收系数达到105 cm-1,且随着掺Fe比例增加而增加.未掺杂的薄膜的光学带隙约为1.6 eV,掺Fe薄膜的禁带宽度接近1.8 eV.     

脉冲偏压及退火处理对电弧离子镀N掺杂TiO_2薄膜结构和性能的影响

本文利用电弧离子镀技术,施加不同脉冲偏压,在玻璃基体上沉积了N掺杂TiO2薄膜。研究了基体偏压和热处理对薄膜结构、光吸收性能及光催化降解甲基橙的反应活性。结果表明:随脉冲偏压的提高,薄膜相结构先由锐钛矿向非晶转变然后向锐钛矿和金红石的混合相转变,吸收边先红移后蓝移,透明度先下降后升高。400℃下退火4 h,薄膜结晶形貌更加明显,吸收边进一步红移,透明度提高。原始薄膜和退火后的薄膜都具有高的紫外光催化活性。可见光下经过退火的-300V偏压下制备的薄膜具有最好的光催化活性。     

不同沉淀剂下水解法制备BiOCl的光催化性能研究

以Bi(NO3)3·5H2O为原料,乙二醇(ethylene glycol,EG)为溶剂,采用水解法,在不同沉淀剂(NH3·H2O,Na2CO3和CO(NH2)2)条件下制备了BiOCl光催化剂.使用X射线衍射(XRD)、扫描电镜(SEM)、N2物理吸附、紫外可见漫反射(DRS)、光致发光(PL)光谱等手段对所制样品进行了表征.以甲基橙染料为降解物,评价了不同沉淀条件对BiOCl光催化性能的影响.结果表明,不同沉淀条件对BiOCl光催化剂的结晶度、晶粒尺寸、形貌、禁带宽度、光生电子空穴对分离效率有明显的影响,进而影响了其光催化活性.其中以尿素为沉淀剂制得的催化剂BiOCl-3在模拟太阳光下降解甲基橙(MO)实验中显示了良好的光催化效率,光照60 min后对MO的降解效率达97;.BiOCl-3较高的光催化活性是由于其具有较高的结晶度、均匀的片状结构、较窄的带隙(2.9 eV)和较高的光生电子-空穴对分离效率.自由基和空穴捕获实验证明,光生空穴是BiOCl-3光催化反应体系中的主要活性物种.此外,所制备的BiOCl-3光催化剂具有较高的光催化稳定性,重复使用4次后对甲基橙的降解率仍保持在89;以上.     

热处理对稀磁半导体Al1-xCuxN薄膜性能的影响

采用磁控溅射法,在蓝宝石衬底上沉积Al1-xCuxN薄膜样品,并对样品进行退火处理.利用X-射线衍射仪和超导量子干涉仪分别研究了退火前后薄膜的结构和磁性能.研究发现退火处理工艺有效地改善了样品的结晶特性和铁磁性:Al1-xCuxN从非晶薄膜转变为多晶薄膜;950℃、氮气气氛退火处理后样品的最大饱和磁矩增加到原来的两倍,约为5.16 emu/cm3.结合X射线光电子能谱和光致发光性能分析,Al1-xCuxN铁磁性来源于Cu原子与其最近邻的N原子之间的p-d杂化和N原子周围缺陷位置极化共同作用.     

不同衬底制备硅薄膜的微结构研究

本文用等离子体增强化学气相沉积(PECVD)技术,在普通玻璃衬底、未织构的氧化锌掺铝(AZO)覆盖的普通玻璃衬底和石英衬底上室温下制备了微晶硅薄膜.然后用快速光热退火炉(RTP)在600℃下对样品进行了7min的退火处理, 借助Raman和SEM对退火前后硅薄膜微结构进行了研究,并用声子限域理论和纳晶表面效应对实验现象进行了分析.结果表明:(1) 薄膜沉积过程中,衬底结构对薄膜微结构有重要影响,相对来说石英衬底上沉积的硅薄膜最容易晶化,其次是玻璃衬底,再其次是未织构的AZO覆盖的玻璃衬底.初步分析认为,主要是因为衬底的无序结构与硅的晶体结构的失配程度不同造成的影响;(2)退火后,薄膜晶粒尺寸均增大.进一步推测, AZO薄膜微结构随退火的变化将导致硅薄膜微结构受到牵连影响.     

Low-temperature fabrication and photocatalytic activity of clustered TiO2 particles formed on glass fibers

Clustered anatase phase TiO₂ particles were uniformly formed on the surface of glass fibers by a liquid phase deposition (LPD) method at 60 °C using TiF₄ and H₃BO₃ as the precursors. The clustered TiO₂ particles deposited on the glass fibers and as a photocatalyst these particles not only have a larger surface area than TiO₂ thin films, but also can avoid the disadvantages of using TiO₂ powders encountered in air purification or water treatment. The photocatalytic activity of the sample was evaluated by the photocatalytic oxidation of nitrogen monoxide (NO) in the gaseous phase. The deposition conditions and chemical composition of the clustered TiO₂ particles were discussed. It was found that the clustered TiO₂ particles that formed on the glass fibers obviously showed photocatalytic activity without high-temperature calcination. A formation mechanism was proposed to account for the formation of TiO₂ clustered morphology on the glass fibers.     

Substrate effect on microstructure and optical performance of sputter‐deposited TiO2 thin films

This study deals with the role of the different substrates on the microstructural, optical and electronical properties of TiO₂ thin films produced by conventional direct current (DC) magnetron sputtering in a mixture of pure argon and oxygen using a Ti metal target with the aid of X–ray diffractometer (XRD), ultra violet spectrometer (UV–vis) and atomic force microscopy (AFM) measurements. Transparent TiO₂ thin films are deposited on Soda lime glass, MgO(100), quartz and sitall substrates. Phase purity, surface morphology, optical and photocatalytic properties of the films are compared with each other. It is found that the amplitude of interference oscillation of the films is in a range of 77‐89%. The transmittance of the film deposited on Soda lime glass is the smallest while the film produced on MgO(100) substrate obtains the maximum transmittance value. The refractive index and optical band gap of the TiO₂ thin films are also inferred from the transmittance spectra. The results show that the film deposited on Soda lime glass has the better optical property while the film produced on MgO(100) substrate exhibits much better photoactivity than the other films because of the large optical energy band gap. As for the XRD results, the film prepared on MgO(100) substrate contains the anatase phase only; on the other hand, the other films contain both anatase and rutile phases. Furthermore, AFM images show that the regular structures are observed on the surface of all the films studied. (© 2012 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

磁控溅射（TiO2-ZnO）/TiO2梯度复合薄膜的制备及光致亲水性研究

采用磁控溅射离子镀设备制备了(TiO2-ZnO)/TiO2梯度复合薄膜,通过TEM、AFM、Raman、XPS分析了复合薄膜的结构、形貌和表面羟基含量,以甲基橙作为有机降解物,研究了(TiO2-ZnO)/TiO2梯度复合薄膜与普通TiO2-ZnO复合薄膜和TiO2薄膜在光催化性能和光致亲水性能上的差异。结果表明:(TiO2-ZnO)/TiO2梯度复合薄膜具有以主体为TiO2-ZnO层、顶层为TiO2的梯度结构,且薄膜表面致密、粒径均匀(10～14 nm),光催化性和亲水性均优于普通TiO2-ZnO复合薄膜和TiO2薄膜,且其光波响应范围红移至450 nm、表面羟基含量高达12.53%,同时梯度复合薄膜的抗光腐蚀性能良好,4 h以后其润湿角仍保持不变。     

Polymer dye-containing nanocomposites as photocatalysts

A significant improvement of photocatalytic efficiency is achieved by the synthesis of TiO₂/SiO₂ nanocomposites where silica matrix provides the transport of reagents to TiO₂ nanoparticles via porous structure, generation of the new active sites and thermal stability. The semiconductive films contained 10 or 30% of TiO₂ in silica matrix are synthesized by sol-gel method using concentrated anatase titania colloid. The complex composites consisted of i) the Acridine Yellow dye molecules and the polyepoxypropyl carbazole; ii) the azobenzene containing polymer covered onto the titania/silica films are obtained as photocatalytic materials. Photocatalytic activity of the composites is tested via the reduction of dichromate ions.     

硫化时间对CuInS2薄膜微结构的影响

采用磁控溅射技术在镀Mo玻璃基片上沉积Cu-In金属预制膜后在N2气氛下硫化制备CuInS2薄膜。研究热处理硫化时间对CuInS2薄膜的表面形貌和晶相结构性能的影响。利用场发射扫描电镜(FE-SEM)、X射线衍射(XRD)和Raman光谱等测试手段对薄膜的表面形貌和晶相结构进行表征。实验结果表明,采用磁控溅射金属预制膜经适当的时间硫化所制备的CuInS2薄膜为黄铜矿结构,随着硫化时间的增加,CuInS2薄膜的晶粒的形貌由球形结构向片状结构转化,并且硫化时间越长,所得薄膜的结晶性能越好,但过长的硫化时间会生成Cu-Au相而导致薄膜质量的劣化。     

Formation of microcrystalline structure in a-Si:H films prepared by RF sputtering

Formation of microcrystalline structure in a-Si:H films prepared by RF sputtering has been investigated by TEM and FT-IR. The Films deposited in pure H₂ have grain-like structure and tend to crystallize with increasing the gas pressure, while the films deposited in Ar containing 10 % H₂ usually become amorphous. With increasing input power and the gas pressure, however, the latter films tend to have amorphous-microcrystalline mixed structure, and corresponding to this structural change, shift of optical absorption edge to lower energy and decreases of resistivity and activation energy of its temperature dependence are observed.     

Effect of deposition pressure on microstructure and properties of hydrogenated carbon nitride films prepared by DC-RF-PECVD

Hydrogenated carbon nitride (a-CN:H films) were deposited on n-type (1 0 0) silicon substrates making use of dual direct current radio frequency plasma enhanced chemical vapor deposition (DC-RF-PECVD), at working pressure of 2–20 Pa, using a mixed gas of CH₄ and N₂ as the source gas. The growth rate, composition, bonding structure of the deposited films were characterized by means of XPS and FTIR, and the mechanical properties of the deposited films were investigated by nano-indentation test. It was found that the parameters for the DC-RF-PECVD process had significant effects on the growth rate, structure and properties of the deposited films. The growth rate of the deposited films increased at first with increasing deposition pressure, then saturated with further increase of the deposition pressure. The N/C ratio inside the deposited films increased with increasing working pressure except that it was as much as 0.50 at a working pressure of 5.0 Pa. The nano-hardness of the films decreased with increasing deposition pressure. CN radicals were remarkably formed in the deposited films at higher pressures, and their contents are related to the nitrogen concentrations in the deposited films.     

Effect of annealing and composition on crystal structure,surface morphology and optical absorption of chemically deposited Cd1‐xSnxS films

Cd_1‐xSn_xS thin films were successfully deposited on suitably cleaned glass substrate by chemical bath deposition method at 74 °C. Hydrated Stannous Chloride (SnCl₂.2H₂O) in aqueous solution was added to the CdS growing solution in different proportions. The experimental results indicate, a successful doping for lower concentration of Sn, saturation for intermediate doping levels, and a degradation of the doping process for higher concentration of Sn. Indirect (X‐ray diffraction) and Direct (Scanning electron microscopy) measurements were performed to characterize the growth and the nature of crystallinity of the different Cd_1‐xSn_xS films. The effect of annealing on the crystal structure and morphology of the deposited films has also been discussed. The X‐ray diffraction spectra show that the thin films are polycrystalline and have both cubic and hexagonal structure. The Interplanar spacing, lattice constant, grain size, strain, and dislocation density were calculated for as‐deposited and annealed films. The grain size was found to decrease from 5 nm to 0.89 nm with doping concentration of Sn. The grain size further decreased due to annealing at 400 °C. SEM studies show layered growth and long needle like structures along with some voids. After annealing the densification and smaller size of the particles was also observed. The optical absorption spectra show shifting of absorption peaks towards lower wavelength side (© 2010 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of the substrate temperature on the crystallization of TiO2 films prepared by DC reactive magnetron sputtering

Titanium oxide (TiO₂) films were deposited on silicon substrates at the temperature in the range 50–600 °C by DC reactive magnetron sputtering. It was found that the anatase and rutile phases co-existed in the TiO₂ films deposited at 450–500 °C, while only the anatase phase existed in those deposited at other temperatures. The mechanism of such a crystallization behavior of TiO₂ films is preliminarily explained.     

纳米TiO2薄膜的制备与光催化性能研究

以四氯化钛为前驱体,采用水解沉淀法,在不同的水解温度下,在硅藻土基多孔陶瓷上负载纳米TiO2薄膜,结合XRD和TEM对负载的纳米TiO2粒径进行了表征。对比分析了测试方法及水解温度对纳米TiO2粒径的影响。以罗丹明B为目标降解物,考察了水解温度对光催化剂活性的影响。结果表明:样品经550℃煅烧后,TiO2薄膜为锐钛矿型;水解温度为50℃时TiO2粒径小于水解温度为75℃时所负载纳米TiO2粒径;两种方法所测TiO2粒径有一定差异:dXRD>dTEM;水解温度为50℃所负载纳米TiO2薄膜,紫外光照300 min,对罗丹明B的去除率为89.9%,而75℃时,样品在紫外光照330 min,对罗丹明B的去除率为78.6%。