直流三极溅射法制备CuInS2 薄膜

采用直流三极溅射装置制备获得了CuInS₂薄膜, 其中溅射靶采用一定面积比的[Cu]/[In]混合靶,反应气体采用CS₂气体. 本文中主要研究了0.02 Pa分压反应气体条件下不同面积比的[Cu]/[In]混合靶和沉积基板温度对CuInS₂薄膜结构和成分的影响, 其中CuInS₂薄膜制备所用时间为2 h生长的厚度为1—2 μm. 通过对CuInS₂薄膜的EPMA, X射线衍射测试分析表明, 最佳的CuInS₂薄膜可在面积比[Cu]/[In]混合靶为1.4:1和可控温度(150, 250和350 ℃)的条件下制备获得, 并且其结构被确认为黄铜矿结构. 通过实验结果计算出CuInS₂薄膜层有约为8.9%的C杂质含量.     

柠檬酸用量对制备纳米晶CaMnO3粉末的影响

 柠檬酸的用量将影响CaMnO₃粉末性能。以金属硝酸盐为原料,去离子水和乙二醇为溶剂,在不同柠檬酸络合剂用量的情况下,采用溶胶 凝胶法制备了CaMnO₃溶胶。通过煅烧干凝胶前驱物制得了钙钛矿型CaMnO₃多晶粉末。利用X射线衍射仪、扫描电子显微镜、激光粒度分析仪等手段分析了所得粉末。结果表明：所得钙钛矿型CaMnO₃晶粒度在20～50 nm之间,粉末为300～500 nm 多边形颗粒,粒度随柠檬酸用量增加而增大,晶粒尺寸也逐渐增大,增幅均较小。     

通过氧化物前驱体非真空方法制备高质量CuInSe2薄膜

通过非真空工艺利用CuO、In₂O₃混合氧化物制备CuInSe₂薄膜太阳能电池中的吸收层CuInSe₂薄膜. 利用柠檬酸法制备出粒径在100 nm以下的CuO、In₂O₃混合氧化物纳米粉,在浆料中加入过量的硒,用来创造非平衡的反应条件促进氧化物的还原和硒化. 考察了影响硒化的几个反应条件,最优的硒化条件为1.9 kPa的Se蒸汽压中,550 °C硒化60 min.     

使用金属掺杂SnO2(110)作为表面催化剂的电催化CO2还原反应：通过调控Sn:O原子比例来控制产物

电催化CO₂还原反应可以产生HCOOH和CO,目前该反应是将可再生电力转化为化学能存储在燃料中的最有前景的方法之一. SnO₂作为将CO₂转换为HCOOH和CO的良好催化剂,其反应发生的晶面可以是不同的. 其中(110)面的SnO₂非常稳定,易于合成. 通过改变SnO₂(110)的Sn:O原子比例,得到了两种典型的SnO₂薄膜：完全氧化型(符合化学计量)和部分还原型. 本文研究了不同金属(Fe、Co、Ni、Cu、Ru、Rh、Pd、Ag、Os、Ir、Pt和Au)掺杂的SnO₂(110),发现在CO₂还原反应中这些材料的催化活性和选择性是不同的. 所有这些变化都可以通过调控(110)表面中Sn:O原子的比例来控制. 结果表明,化学计量型和部分还原型Cu/Ag掺杂的SnO₂(110)对CO₂还原反应具有不同的选择性. 具体而言,化学计量型的Cu/Ag掺杂的SnO₂(110)倾向于产生CO(g),而部分还原型的表面倾向于产生HCOOH(g). 此外,本文还考虑了CO₂还原的竞争析氢反应. 其中Ru、Rh、Pd、Os、Ir和Pt掺杂的SnO₂(110)催化剂对析氢反应具有较高的活性,其他催化剂对CO₂还原反应具有良好的催化作用.     

衬底对原位氧化制备的ZnO薄膜结构和光学性质的影响

 采用射频反应溅射法在不同衬底上制备Zn₃N₂薄膜,然后对其原位氧化制备ZnO薄膜。利用X射线衍射分析(XRD)、扫描电子显微镜(SEM)和光致发光谱(PL)等表征技术研究了不同衬底对ZnO薄膜的结晶特性和发光性能的影响。XRD研究结果显示:Zn₃N₂薄膜在500 ℃原位氧化3 h后完全转变为ZnO薄膜,在玻璃和熔融石英衬底上制备的多晶ZnO薄膜无择优取向,而单晶硅（100）衬底上的多晶ZnO薄膜具有较好的沿（002）方向的择优取向。PL测试结果显示:硅和熔融石英衬底上的多晶ZnO薄膜发光性能良好,激子复合产生的紫外发光峰很强,且半高宽较窄,而来自于深能级发射的绿色发光峰很弱;而玻璃衬底上的多晶ZnO薄膜发光性能较差。     

不同前驱体相对摩尔量对气相爆燃制备纳米SiO2的影响

 以SiCl₄为前驱体,以空气和氢气的混合气体为爆源,通过改变前驱体的相对摩尔量,考察前驱体的相对摩尔量对产物的影响。通过X射线荧光谱（XRF）、透射电子显微镜（TEM）和X射线衍射（XRD）等测试手段对纳米SiO₂粉体进行表征及分析。通过XRF对产物进行成分分析,测得实验所得产物主要由SiO₂组成,且纯度达到99.9%以上;由XRD分析得知,生成的SiO₂产物属于典型的非晶态结构;由TEM图像可以看出,随着前驱体相对摩尔量的增加,所得到的产物粒子逐渐出现粘结,分散性下降,前驱体相对摩尔比应该控制在1.5以内。     

Zn掺杂β-Ga2O3薄膜的制备和特性研究

β-Ga₂O₃是一种宽带隙半导体材料,能带宽度E_g≈5.0eV,在光学和光电子学领域有广泛的应用。用射频磁控溅射方法在Si衬底和远紫外光学石英玻璃衬底制备了本征β-Ga₂O₃薄膜及Zn掺杂β-Ga₂O₃薄膜,用紫外 可见分光光度计、X射线衍射仪、荧光分光光度计对本征β-Ga₂O₃薄膜及Zn掺杂β-Ga₂O₃薄膜的光学透过、光学吸收、结构和光致发光进行了测量,研究了Zn掺杂和热退火对薄膜结构和光学性质的影响。退火后的β-Ga₂O₃薄膜为多晶结构,与本征β-Ga₂O₃薄膜相比,Zn掺杂β-Ga₂O₃薄膜的β-Ga₂O₃(111)衍射峰强度变小,结晶性变差,衍射峰位从35.69°减小至35.66°。退火后的Zn掺杂β-Ga₂O₃薄膜的光学带隙变窄,光学透过降低,光学吸收增强,出现了近边吸收,薄膜的紫外、蓝光及绿光发射增强。表明退火后Zn掺杂β-Ga₂O₃薄膜中的Zn原子被激活充当受主。     

三维海胆状Co3O4的微纳结构制备及锂电池性能

水热法制备的合成海胆状Co₃O₄前驱物在空气中退火得到三维海胆状Co₃O₄的微纳结构. 采用FESEM、TEM、HRTEM以及XRD对产物进行形貌和结构的表征. 结果表明,合成的海胆状结构Co₃O₄由许多粒径约为15 nm的颗粒串接形成. 锂电池测试性能表明,制备的海胆状Co₃O₄首次放电容量达到1.369 Ah/g,经过20次循环     

不同[Cu]/[In]比例的CuInS2薄膜的特性

采用连续离子层吸附与反应方法在玻璃基板上按照不同[Cu]/[In]的比例制备了CuInS₂薄膜,并在400 °C退火30 min. 对薄膜的晶体结构和晶粒尺寸用X射线衍射方法进行了表征,原子力显微镜测定薄膜的表面形貌. 研究不同的[Cu]/[In]比例对薄膜光学和电学性能的影响. 采用直流两探针法在300～470 °C测定CuInS₂薄膜的电阻率,随着[Cu]/[In]比例的增加,电阻率值越来越低. 溶液中[Cu]/[In]的比例明显影响CuInS₂薄膜的结构、电学和光学特性.     

多层膜外退火方法制备MgB2超导薄膜

报道了利用电子束蒸发的Mg/B多层膜作为前驱体，然后退火制备MgB₂薄膜的工作. 实验中发现，采用翻转膜面的退火处理方式可以有效地避免降温过程中Mg蒸气在薄膜表面形成的颗粒凝结，由此稳定地实现了面积为10 mm×10 mm，均匀、平整的超导薄膜的制备，T_c达35 K，转变宽度为0.8 K，在5 μm×5 μm的区域内薄膜的平均粗糙度小于10 nm. 为了便于后续器件制作过程中的微加工工艺，研究了膜厚小于1000 ?时薄膜的成相规律，发现当样品厚度减薄后，T_c会有明显降低. 通过调整前驱薄膜中的不同分层厚度，仍可实现转变温度达30 K以上、厚度约600 ?的MgB₂薄膜，在20 K时的临界电流密度为2.4×10⁶ A/cm².     

Structural and optical characterization of Sb-doped CuInS2 thin films grown by vacuum evaporation method

Structural, electrical and optical properties of Sb-doped CuInS₂ thin films grown by single source thermal evaporation method were studied. The films were annealed from 100 to 500 °C in air after the evaporation. The X-ray diffraction spectra indicated that polycrystalline CuInS₂ films were successfully obtained by annealing above 200 °C. This temperature was lower than that of non-doped CuInS₂ films. Furthermore, We found that the Sb-doped CuInS₂ thin films became close to stoichiometry in comparison with non-doped CuInS₂ thin films. The Sb-doped samples annealed above 200 °C has bandgap energy of 1.43–1.50 eV.     

Effect of [Cu]/[In] ratio on properties of CuInS2 thin films prepared by successive ionic layer absorption and reaction method

CuInS₂ ternary films were prepared by a soft solution processing, i.e. successive ionic layer absorption and reaction (SILAR) method. The films were deposited on glass substrates at room temperature and heat-treated under Ar atmosphere at 500 °C for 1 h. CuCl₂ and InCl₃ mixed solutions with different ionic ratios ([Cu]/[In]) were used as cation precursor and Na₂S as the anion precursor. The effect of the [Cu]/[In] ratio in precursor solution on the structural, chemical stoichiometry, topographical, optical and electrical properties of CuInS₂ thin films was investigated. XPS results demonstrated that stoichiometric CuInS₂ film can be obtained by adjusting [Cu]/[In] ratios in solution. Chalcopyrite structure of the film was confirmed by XRD analysis. The near stoichiometric CuInS₂ film has the optical band gap E_g of 1.45 and resistivity decreased with increase of [Cu]/[In] ratios.     

Real-time study of phase transformations in Cu-In chalcogenide thin films using in situ Raman spectroscopy and XRD

The growth of polycrystalline CuInSe₂ and CuInS₂ thin films from metallic precursor layers is investigated using two complementary in situ methods which give bulk sensitive (XRD) and surface sensitive (Raman) information. From the time evolution of the XRD and Raman peak intensities the phase transformation sequences and the reaction kinetics can be derived. In both cases the chalcogenization of the Cu-In precursors proceeds at the top surface. Thus, the process is at least limited by cation diffusion through the metallic precursor. However, the growth kinetics of CuInSe₂ and CuInS₂ films differ. While the CuInSe₂ growth is limited by the reaction of binary phases, CuInS₂ growth is controlled by fast diffusion which is solely restricted to the period of raising temperature during the process.     

Improvement in efficiency of solar cell by removing Cu2－xSe from CIGS film surface

CIGS thin films are deposited by sputtering and selenization. The synthesis of semiconducting polycrystalline thin films and characteristics of devices based on the CIGS absorbing layers are investigated. Their microstructures are characterized by x-ray diffraction and Raman spectroscopy. The results reveal that there exist metallic Cu_2-xSe compounds in CIGS film surfaces and the compounds are thought to be responsible for the degradation of the open circuit voltage of solar cells. The optimization of selenization temperature profile and copper content in the precursor surfaces is studied, concluding that the conversion efficiency may be improved by removing metallic Cu_2-xSe compounds from the surfaces of CIGS thin films.     

Properties of CuIn(SxSe1−x)2 polycrystalline thin films prepared by chemical spray pyrolysis

CuIn(S_xSe_1−x)₂ thin polycrystalline films were grown by the chemical spray pyrolysis method on the glass substrate at 280-400°C. The alloy composition in the film was studied with relation to that in the splay solution. Films were characterized by X-ray diffraction, optical absorption, Raman spectroscopy, resistivity and surface morphology. The CuInSe₂-rich alloy films grown at high substrate temperature had chalcopyrite structure, while, the CuInS₂-rich films grown at low substrate temperature exhibited sphalerite structure. Optical-gap energies were smaller than that of the bulk crystal by 0.1-0.2 eV for CuInS₂-rich films. Raman spectra exhibited both CuInSe₂-like and CuInS₂-like A₁ modes, and their relative changed systematically with alloy composition.     

Fabrication of nanostructured CuInS2 thin films by ion layer gas reaction method

CuInS₂ thin films were prepared by a two-stage ion layer gas reaction (ILGAR) process in which the Cu and In precursors were deposited on glass substrate by using a simple and low-cost dip coating technique and annealed in H₂S atmosphere at different temperatures. The influence of the annealing temperature (250-450 °C) on the particle size, crystal structure and optical properties of the CuInS₂ thin films was studied. Transmission electron microscopy revealed that the particle radii varied in the range 6-21 nm with annealing. XRD and SAED patterns indicated polycrystalline nature of the nanoparticles. The optical band gap (E_g) varied from 1.48 to 1.56 eV with variation of particle size. The variation of Urbach tail with temperature indicated higher density of the defects for the films annealed at lower temperature. From the Raman study, it was observed that the FWHM of the A₁ mode at ∼292 cm⁻¹ corresponding to the chalcopyrite phase of CuInS₂ decreased with increasing annealing temperature.     

Effect of ultrasonic irradiation on structure and electrochemical properties of LiMn2O4 thin films cathode material for Li-ion micro-batteries

Two kinds of spinel LiMn₂O₄ thin film for lithium ion micro-batteries were successfully prepared on polycrystal Pt substrates by spin coating methods, which were carried out under ultrasonic irradiation (USG) and magnetic stirring (MSG), respectively. The microstructures and electrochemical performance of LiMn₂O₄ thin films were characterized by thermogravimetry analysis (TGA), X-ray diffraction (XRD), scanning electron microscopy (SEM), and galvanostatic charge-discharge measurements. It was found that the crystalline structure of USG samples grew better than that of the MSG samples. At the same time, higher discharge capacity and better cycle stability were obtained for the LiMn₂O₄ thin films of USG at the current density of 50 μAh/cm² between 3.0 and 4.3 V. The 1st discharge capacity was 57.8 μAh/cm²-μm for USG thin films and 51.7 μAh/cm²-μm for MSG thin films. After 50 cycles, 91.4% and 69% of discharge capacity could be retained respectively, indicating that ultrasonic irradiation condition during spin coating was more suitable for preparing spinel LiMn₂O₄ thin films with better electrode performance for lithium ion micro-batteries.     

Preparation and photo-induced superhydrophilicity of composite TiO2-SiO2-In2O3 thin film

In this work, TiO₂-SiO₂-In₂O₃ composite thin films on glass substrates were prepared by the sol-gel dip coating process. X-ray diffraction (XRD), X-ray fluorescence spectroscopy (XRF) and X-ray photoelectron spectroscopy (XPS) were used to evaluate the structural and chemical properties of the films. UV-vis spectrophotometer was used to measure the transmittance spectra of thin films. The water contact angle (WCA) of thin films during UV/vis irradiation and storage in a dark place was measured by a contact angle analyzer. The results indicated that fabrication of composite film has a significant effect on transmittance and superhydrophilicity of TiO₂ films.     

Influence of annealing temperature on properties of Cu(In,Ga)(Se,S)2 thin films prepared by co-sputtering from quaternary alloy and In2S3 targets

Pentanary Cu(In,Ga)(Se,S)₂ (CIGSS) thin films were deposited on soda-lime glass substrate by co-sputtering quaternary alloy, and In₂S₃ targets. In this study, we investigated the influence of post-annealing temperature on structural, compositional, electrical, and optical properties of CIGSS films. Our experimental results show that the CIGS quaternary target had chalcopyrite characteristics. All CIGSS films annealed above 733 K exhibited a polycrystalline tetragonal chalcopyrite structure, with (1 1 2) preferred orientation. The carrier concentration and resistivity of the resultant CIGSS layer annealed above 763 K was 4.86×10¹⁶ cm⁻³ and 32 Ω cm, respectively, and the optical band-gap of the CIGSS absorber layer was 1.18 eV. Raman spectral analysis demonstrated the existence of many different phases, including CuInSe₂, CuGaSe₂, and CuInS₂. This may be because the vibration frequencies of In-Se, In-S bonds are similar to the Ga-Se and Ga-S bonds, causing their absorption bands overlap.