CuInSe<Subscript>2</Subscript> thin films obtained by pulse-plating electrodeposition technique with novel pulse wave

CuInSe₂ films were electrodeposited onto indium tin oxide (ITO) substrate in constant current mode using bell-like wave modulated square wave in aqueous solution. The films obtained at different pulse frequencies were characterized by scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). UV-Vis-NIR absorption spectro- scopy was used to study the optical properties of these films. The results showed that the chalcopyrite phase CuInSe₂ films with a smooth surface and stoichiometric composition could be obtained at appropriate pulse frequency. The crystallinity of CuInSe₂ films could be further improved after annealing treatment. Despite this, we also found that the films obtained using the pulse-plating electrodeposition technique had a faster deposition rate and better film adhesion ability than that using the traditional CIS elec-trodeposition technique, which is significant to the low-cost CIS thin film solar cell production.     

双源法制备CuInSe2多晶薄膜的研究

利用氮气作保护气体，用元素合成法进行开管烧结，合成具有单一相黄铜矿结构的CuInSe     

Synthesis of the CuInSe2 thin film for solar cells using the electrodeposition technique and Taguchi method

The Taguchi method was used to obtain the optimum electrodeposition parameters for the synthesis of the CuInSe₂ thin film for solar cells. The parameters consist of annealing temperature, current density, CuCl₂ concentration, FeCl₃ concentration, H₂SeO₃ concentration, TEA amount, pH value, and deposition time. The experiments were carried out according to an L₁₈(2137) table An X-ray diffractometer (XRD) and a scanning electron microscope (SEM) were respectively used to analyze the phases and observe the microstructure and the grain size of the CuInSe₂ film before and after annealing treatment. The results showed that the CuInSe₂ phase was deposited with a preferred plane (112) parallel to the substrate surface. The optimum parameters are as follows: current density, 7 mA/cm 2 ; CuCl₂ concentration, 10 mM; FeCl₃ concentration, 50 mM; H₂SeO₃ concentration, 15 mM; TEA amount, 0 mL; pH value, 1.65; deposition time, 10 min; and annealing temperature, 500℃.     

电沉积和硒化制备CuInSe2薄膜

以石墨为阳极、钛片为阴极,采用恒电流法制备Cu-In预制膜,然后硒化处理得到CuInSe2薄膜.分析了预制膜和CuInSe2薄膜的相组成及其影响因素.结果表明:采用不同的电沉积工艺,可以得到不同相组成的Cu-In预制膜.在保证Cu/In小于1的条件下,降低InCl3浓度和H3Cit/CuCl2浓度比,选择较高电流,可以获得具有CuIn相和Cu2In相的Cu-In预制膜.含有CuIn相和Cu2In相的Cu-In预制膜,经硒化得到的CuInSe2薄膜具有单一CuInSe2相组成,并且符合化学剂量比要求;而只含有CuIn相的预制膜硒化后除了有CuInSe2相外还出现了CuSe相.     

Preparation and magnetic properties of CoFe2O4/TiO2 composite films

Using （Ti（OC4H9）4） and metal chlorates as starting materials, CoFe2O4/TiO2 composite films were prepared by sol-gel method. The effects of heat treatment temperature and pH of the precursor on microstructure and magnetic properties were studied. The phase structure of the samples was examined by X-ray diffraction. The microstructure was examined by scanning electron microscope, atomic force microscope and polarized microscope. The magnetic property was measured by vibrating sample magnetometer. The results show that the crystals of different phases grow up independently. CoFe2O4 is uniformly embedded into the TiO2 matrix in the prepared composite films, and the growth of composite films is dependent on the heat treatment temperatures and PH of the precursor. The average size of CoFe2O4 crystal is 19 nm in Nanocomposite film prepared when the heat treatment temperature is 800℃ and the pH of the precursor is between 2 and 3. The magnetism of the composite films is enhanced as the heat treatment temperature increases.     

Cu-In膜的相结构对CuInSe2薄膜性能的影响

为考察溅射功率对Cu-In薄膜中相结构以及相应的CuInSe2(简称CIS)薄膜性能的影响,采用中频交流磁控溅射方法沉积Cu-In薄膜,并采用固态硒化方法形成CIS薄膜.采用SEM和EDX观察和分析了它们的表面形貌和成分,采用XRD表征了薄膜的组织结构,并分析了硒化中的反应动力学过程.结果表明,在不同的溅射功率条件下,Cu-In预制膜以Cu11In9相或Cu11In9和CuIn的混合相存在.由Cu11In9和CuIn混合相薄膜形成的CIS薄膜具有单一的CuInSe2相黄铜矿相结构,且其成分接近CuInSe2化学计量比.而由Cut1In9相Cu-In预制膜形成的CIS薄膜中除了CuInSe2相以外,还出现了Cu2Se相,且其成分远离CuInSe2化学计量比.因此,具有Cu11In9和CuIn混合相结构的CuIn薄膜更适合制备CIS太阳电池吸收层.     

硒化法制备铜铟铝硒薄膜及其性能研究

采用中频交流磁控溅射方法制备了CIA前驱膜,并采用固态硒化法进行处理,获得了CIAS吸收层薄膜。采用SEM和XRD观察和分析了薄膜的成分、组织结构和表面形貌。结果表明,通过调节CIA前驱膜的Al含量可制备得到Cu/(In Al)原子比接近1,且Al/(In Al)比例可调的CIAS薄膜。CIAS薄膜由Cu(In1-xAlx)Se2固溶体相组成,Al主要是以替代In的固溶形式存在。     

准东高铁煤与稻草秆热解NOx前驱物释放规律研究

氨(NH_3)和氰氢酸(HCN)是燃料热解过程中的主要含氮化合物,也是燃烧过程中重要的NO_x前驱物,因此研究热解过程中HCN/NH_3的释放规律与转化机制,对降低NO_x排放意义重大。借助热重-质谱联用(TG-MS)系统开展实验研究,探讨了准东高铁煤与稻草秆热解过程中NO_x前驱物的释放规律。研究表明:准东高铁煤与稻草秆的热解产物中,NH_3是主要的NO_x前驱物;NH_3与HNCO、HCN与CH_3CN的释放规律趋同;同等实验条件下,稻草秆热解的NO_x前驱物释放量明显高于准东高铁煤的;准东高铁煤与稻草秆混合热解时,当稻草杆掺混质量百分比从10%增加至40%时,NO_x前驱物的释放量呈先减少后增加的趋势,NO_x前驱物释放量最低时的掺混比为30%,说明稻草秆与准东高铁煤共热解时,二者对NO_x前驱物的释放具有一定的协同耦合抑制作用。     

Bi_(1.6)La_(0.4)Ti_2O_7薄膜的制备及性能研究

采用化学溶液沉积法在ITO基片上制备不同退火温度的掺镧钛酸铋Bi1.6La0.4Ti2O7(BLT)薄膜。研究了其结构、介电性能、漏电流密度与外加电压I-V关系曲线和光学带隙。XRD射线衍射测试结果表明,经500、550、600℃1 h退火后的薄膜的主晶相为烧绿石结构,无杂相生成,600℃时BLT薄膜衍射峰比其他两种温度的强。在1 kHz频率下测得的介电常数、损耗因子分别为114,3%;129,3%;194,6%。BLT薄膜的漏电流密度与外加电压关系曲线表明,BLT薄膜600℃的漏电流比550和500℃稍微减小。通过透射谱分析得到BLT薄膜的光学带隙几乎不受温度影响,均为3.7 eV。这些结果表明制备BLT固溶体薄膜较佳为退火温度600℃,具有较好的性能,在光电器件有良好的应用前景。     

CeO2 thin films grown on biaxially textured nickel (001)

CeO\-2 films have been grown on biaxially textured Ni substrates at various temperatures. The results show that CeO\-2 films without IBAD are dominated by (111) orientation from room temperature to 800℃ while the preferential orientation of CeO\-2 films with IBAD is (001) at lower deposition temperature and (111) at deposition temperature higher than 450℃. CeO\-2 films with better in_plane texture and out_of_plane orientation can be grown at 360℃ with 240 eV ion energy and 200 μA/cm\+2 ion current density.     

BaAl2S4:Eu溅射靶材合成方法研究

采用放电等离子烧结(SPS)方法和粉末烧结法制备BaAl2S4:Eu溅射靶材,分析了靶材成分和结构特性以及利用靶材制备薄膜的发光特性.实验结果表明,SPS烧结的BaAl2S4:Eu溅射靶材的纯度高,无其它硫化物形成,被氧化的可能性小,靶材致密,气孔少;形成薄膜的PL谱主要是470nm处的蓝光发射.粉末烧结法制备的Ba-Al2S4:Eu溅射靶材的纯度低,靶材被氧化的几率大,气孔多,不致密,呈三维网状结构;在470nm处的蓝光发射峰值相对较弱.放电等离子烧结方法更适合制备BaAl2S4:Eu溅射靶材.     

热处理温度对溶胶-凝胶法制备的Ce_(0.97)Co_(0.03)O_2薄膜结构和光学性能的影响

采用溶胶-凝胶法,在Si(100)衬底上制备了3%Co掺杂CeO2薄膜,研究了不同热处理温度对Ce0.97Co0.03O2薄膜结构和光学性质的影响。X射线衍射(XRD)表明,3%Co掺杂CeO2薄膜为多晶薄膜,且未破坏CeO2原有的结构,随着退火温度的升高,晶粒尺寸逐渐增大。椭偏光谱法研究表明,Ce0.97Co0.03O2薄膜的光学常数(折射率n、消光系数k)随着退火温度增加而增大,光学带隙Eg随退火温度增加而减小,这是薄膜结构随退火温度增加发生变化所致。     

Photoinduced effects in amorphous semiconductor Ge(S, Se)2 chalcogenide films

The blue shift of optical transmittance edges were observed in amorphous semiconductor Ge(S, Se)₂ chalcogenide films with light illumination. The shift in well-annealed films could be recovered by annealing the films near the glass-transition temperature again. The photocrystallization was also observed in amorphous Ge(S,Se)₂ films with light illumination by the transmitting electron microscope measurement. The photoinduced phenomina of the amorphous Ge(S,Se)₂ films could be applied to designing some new kinds of optical storage materials.     

衬底偏压对γ′-Fe4N薄膜磁性的影响

采用直流磁控溅射方法, 以Ar/N₂（N₂/(Ar+N₂)=10％）为放电气体, 在Si(100)单晶衬底上获得了γ′-Fe₄N薄膜样品. 利用X射线衍射(XRD)和振动样品磁强计(VSM)研究衬底偏压对γ′-Fe₄N薄膜样品的影响. 结果表明, 随着衬底负偏压的增大, γ′-Fe₄N薄膜样品的晶胞参数减小, Fe和N的化合效率与样品的致密度提高, 表面缺陷减少, 矫顽力降低.      

磁控溅射表面镀膜对Nd2Fe14B稀土永磁体抗腐蚀性能的影响

在Nd₂Fe₁₄B稀土永磁体基体表面,采用磁控溅射（直流+射频）技术制备了Ti/Ni,Ti/Al和Al/Ni等二元合金薄膜和Ti/Al/Ni三元合金薄膜。并通过中性盐雾试验、腐蚀失重计算、电化学腐蚀试验、金相观察等方式,对比研究了不同表面处理对Nd₂Fe₁₄B稀土永磁体基体抗腐蚀性能的影响,并构建了腐蚀模型。研究发现：Ti/Ni,Ti/Al和Al/Ni等二元合金薄膜和Ti/Al/Ni三元合金薄膜均有效地提高了Nd₂Fe₁₄B稀土永磁体基体耐中性盐雾腐蚀和电化学腐蚀的能力;Ti/Al/Ni三元合金薄膜较Ti/Ni,Ti/Al和Al/Ni等二元合金薄膜有更优良的综合耐腐蚀性能,其磁控溅射工艺参数为：Ar流量60 sccm,基片温度常温,Ni,Al,Ti的溅射功率都为250 W,基片转速20 r·min^-1,镀膜均速0.3 nm·s^-1,总计溅射时间1 h。     

Catalyst enhanced chemical vapor deposition of nano-particle nickel films on teflon surface

Films formed with nanosized nickel particles on teflon surface were prepared by means of catalyst enhanced chemical vapor deposition (CECVD) with Ni(dmg)₂, Ni(acac)₂, Ni(hfac)₂, Ni(TMHD)₂, and Ni(cp)₂ as precursors, and complexes Pd(hfac)₂, PdCl₂ and Pd(η ³-2-methylallyl)acac as catalyst under carrier gas (H₂). The film growth rate depends on the precursors and substrate temperature. The chemical value, purity and surface morphology of the Ni particle films were characterized by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The films obtained were shiny with silvery color, and consisted of grains with a particle size of 50–140 nm. The Ni was metallic of which the purity was about 90%–95% from XPS analysis. SEM micrograph showed that the film had good morphology.      

Silicon field emission arrays coated with CN<Subscript>x</Subscript> thin films

Arrays of silicon micro-tips were made by etching the p-type (1 0 0) silicon wafers which had SiO₂ masks with alkaline solution. The density of the micro-tips is 2×10⁴ cm⁻². The Scanning Electron Microscope (SEM) photos showed that the tips in these arrays are uniform and orderly. The CN_x thin film, with the thickness of 1.27 μm was deposited on the silicon micro-tip arrays by using the middle frequency magnetron sputtering technology. The SEM photos showed that the films on the tips are smoothly without particles. Keeping the sharpness of the tips will benefit the properties of field emission. The X-ray photoelectron spectrum (XPS) showed that carbon, nitrogen and oxygen are the three major elements in the surfaces of the films. The percents of them are C: 69.5%, N: 12.6% and O: 17.9%. The silicon arrays coated with CN_x thin films had shown a good field emission characterization. The emission current intensity reached 3.2 mA/cm² at 32.8 V/μm, so it can be put into use. The result showed that the silicon arrays coated with CN_x thin films are likely to be good field emission cathode. The preparation and the characterization of the samples were discussed in detail. Foundation item: Supported by the National Natural Science Foundation of China (19975035) Biography: Chen Ming an (1978-), male, Ph. D candidate, research direction: novel functional materials film and ion beam modification of materials.     

Structural and electrical properties of ZnO films on freestanding thick diamond films

In this paper, ZnO films are deposited on freestanding thick diamond films （FTDF） by plasma-assisted metal organic chemical vapour deposition （MOCVD）. Diethyl zinc （DEZn）, O2 and N2O are applied as precursors and different substrate temperatures are used to achieve high quality ZnO films. The influence of substrate temperature on the properties of ZnO films is systematically investigated by X-ray diffraction （XRD）, Hall measurements and electron probe microanalysis （EPMA）. Experimental results demonstrate that ZnO films deposited at 600℃ and 73 Pa display a fine electrical quality and Zn/O atomic ratio plays an important role in the electrical property of ZnO films.     

Comparison between P25 and anatase-based TiO<Subscript>2</Subscript> quasi-solid state dye sensitized solar cells

Pure anatase TiO2 films have been made via hydration of titanium isopropoxide using a sol-gel tech-nique, while mixed TiO2 films which contained both anatase and rutile TiO2 were made from commercial P25 powder. Quasi-solid state dye-sensitized solar cells were fabricated with these two kinds of mesoporous films and a comparison study was carried out. The result showed that the open-circuit photovoltages （Voc） for both kinds of cells were essentially the same, whereas the short-circuit photo-currents （1sc） of the anatase-based cells were about 33% higher than that of the P25-based cells. The highest photocurrent intensity of the anatase-based cell was 6.12 mA/cm^2 and that of the P25-based cell was 4.60 mA/cm^2. Under an illumination with the light intensity of 30 mW/cm^2, the corresponding energy conversion efficiency was measured to be 7.07% and 6.89% for anatase-based cells and P25-based cells, respectively.     

TiO2/SiO2/GQDs双层增透膜的制备及其在太阳能板中的应用

采用溶胶-凝胶法制备了SiO₂ 和TiO₂ 纳米溶胶,采用水热法制备了石墨烯量子点（graphene quantum dots,GQDs）。为进一步提高光伏太阳能板的透光率,设计了一种TiO₂/SiO₂/GQDs双层增透膜结构。探究了薄膜的结构、自清洁性能和增透性能,并进一步讨论了GQDs在增透性中的作用。结果表明,SiO₂-TiO₂/TiO₂-GQDs结构的双层薄膜厚度为120 nm时,太阳能板上的光透过率由未涂敷的85%增加至95%。接触角实验和室外耐环境性能实验测试表明,复合膜层接触角为10°,并具有良好的亲水性和耐环境性能。此外,户外实验结果表明,涂覆该薄膜的太阳能电板发电效率提高6%。由此说明双层增透膜可有效地提高太阳能电池板的光能利用率和使用寿命,可高效地利用太阳能。