Synthesis and characterization of type-II textured tungsten disulfide thin films by vdWR process with Pb interfacial layer as texture promoter

The growth of type-II textured tungsten disulfide (WS₂) thin films by solid state reaction between the spray deposited WO₃ and gaseous sulfur vapors with Pb interfacial layer has been studied. X-ray diffraction (XRD) technique is used to measure the degree of preferred orientation ‘S’ and texture of WS₂ films. Scanning electron microscopy (SEM) and transmission electron microscopy techniques have been used to examine the microstructure and morphology. The electronic structure and chemical composition were studied using X-ray photoelectron spectroscopy (XPS). The use of Pb interfacial layer for the promotion of type-II texture in WS₂ thin films is successfully demonstrated. The presence of (0 0 3 l), (where l=1, 2, 3, …) family of planes in the XRD pattern indicates the strong type-II texture of WS₂ thin films. The crystallites exhibit rhombohedral (3R) structure. The large value of ‘S’ (1086) prompts the high degree of preferred orientation as well. The stratum of crystallites with their basal plane parallel to the substrate surface is seen in the SEM image. The EDS and XPS analyses confirm the tungsten to sulfur atomic ratio as 1:1.75. We purport that Pb interfacial layer enhances type-II texture of WS₂ thin films greatly.     

Microstructure and ferroelectric properties of BaTiO3 films on LaNiO3 buffer layers by rf sputtering

We have fabricated LaNiO₃ and BaTiO₃ films using the rf sputtering method. The LaNiO₃ were deposited on Si substrates, demonstrating a (1 0 0) highly oriented structure and nanocrystalline characteristic with a grain size of 30 nm. The BaTiO₃ thin films were deposited on the LaNiO₃ buffer layers, and have exhibited a (1 0 0) texture with a thickness of 400 nm. A smooth interface is obtained between the LaNiO₃ bottom electrode and the BaTiO₃ film from cross-section observations by scanning electron microscopy. The bi-layer films show a dense and column microstructure with a grain size of 60 nm. Ferroelectric characterizations have been obtained for the BaTiO₃ films. The remnant polarization and coercive field are 2.1 μC/cm² and 45 kV/cm, respectively. The leak current measurements have shown a good insulating property.     

射频溅射功率对Mn-Co-Ni-O薄膜结构与性能的影响

采用射频磁控溅射技术在硅衬底上制备了锰钴镍氧(Mn-Co-Ni-O, MCNO)薄膜并进行了后退火处理。利用X射线衍射、扫描电子显微镜、光学测试仪器等测试手段对晶体结构、表面形貌及光学性能进行表征。分析了不同射频溅射功率(60~100 W)对MCNO薄膜表面微观形貌、晶体结构和光学性能的影响。结果表明,在60~90 W下获得的薄膜表面致密且均匀,但在100 W下获得的MCNO薄膜表面晶粒尺寸显著增大。物相分析表明,采用射频磁控溅射沉积的MCNO薄膜主要为尖晶石结构,溅射功率对薄膜结晶质量和择优取向具有显著影响,在80 W下获得的MCNO薄膜结晶质量最佳。同时,拉曼光谱测试也表明该MCNO薄膜表现出最强的Mn⁴⁺—O对称弯曲振动和最小的压应力。紫外-可见-近红外光谱分析表明,MCNO薄膜的吸光范围主要在可见光-近红外波段,在80~90 W溅射功率下获得的MCNO薄膜在近红外波段表现出更强的吸收峰。射频溅射功率的改变会影响薄膜的厚度和结晶质量,从而对薄膜的光学带隙起到调控作用。光致发光光谱测试不同溅射功率下薄膜的缺陷峰发光强度,且在功率为80 W时沉积的薄膜具有最强紫外发射峰,表明改变溅射功率能够有效改善薄膜缺陷及提高晶体质量。     

氧分压调控氧化铜薄膜生长及其表面功函数研究

本文采用反应磁控溅射法制备p型二元铜氧化物半导体薄膜,通过氧气流量调节实现Cu₂O、CuO和Cu₄O₃薄膜的可控生长。所制备薄膜的形貌与结构分别利用扫描电子显微镜、X射线衍射仪以及拉曼光谱进行表征。经紫外可见分光光度计测量可知,Cu₂O、CuO和Cu₄O₃薄膜的带隙分别为2.89 eV、1.55 eV和2.74 eV。为进一步研究Cu₂O、CuO和Cu₄O₃薄膜的表面物理性质,基于Kelvin探针力显微镜(KPFM)技术直接测量了薄膜样品与探针尖端间的接触电位差(V_CPD),结果表明Cu₂O、CuO和Cu₄O₃薄膜的表面功函数都随着温度的升高而呈现逐渐减小的趋势。     

Facile synthesis of ordered large-pore mesoporous silica thin film with Im3m symmetry using n-butanol as the cosurfactant

A facile synthesis route to ordered large-pore (10.7 nm) mesoporous silica film with the cubic Im3m mesostructure is reported in a TEOS–F127–BuOH–HCl–H₂O system through dip-coating method. Characterization by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and nitrogen sorption reveals that the obtain mesoporous silica material possessed high surface area and large pore diameter. A relative comparison between the mesoporous silica films synthesized with and without BuOH is also presented. A reasonable formation mechanism of the large-pore mesoporous silica film is depicted in this work.     

磁控溅射衬底加热温度和后退火温度对制备β-Ga2O3薄膜材料的影响

作为宽禁带半导体材料的一员,结构稳定的β-Ga₂O₃具有比SiC和GaN更宽的禁带宽度和更高的巴利加优值,近年来受到科研人员的广泛关注。本文采用射频(RF)磁控溅射法在C面蓝宝石衬底上生长β-Ga₂O₃薄膜,探究溅射过程中衬底加热温度的影响。溅射完成后通过高温退火处理提升薄膜质量,研究衬底加热温度和后退火温度对氧化镓薄膜晶体结构和表面形貌的影响。利用X射线衍射(XRD)、原子力显微镜(AFM)等测试手段对β-Ga₂O₃薄膜晶体结构、表面形貌等进行分析表征。实验结果表明,随着衬底加热温度的升高,β-Ga₂O₃薄膜表面粗糙度逐渐降低,薄膜晶体质量得到显著提升;在氧气气氛中进行后退火,合适的后退火温度有利于氧化镓薄膜重新结晶、增大晶粒尺寸,能够有效修复薄膜的表面态和点缺陷,对于改善薄膜晶体质量有明显优势。     

Preparation of mesoporous oxide films via block copolymer templating

Mesoporous silica films have been synthesized by a modified sol-gel method in the presence of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) block copolymers as structure-directing agents. Influence of synthetic conditions on the formation of mesoporous silica films has been investigated. Porosity of samples can be controlled by block copolymer concentration and aging time of precursor solutions, while the block length of block copolymers affects mesoporous structures. Post-deposition chemical treatment using vaporized ammonia makes it possible to control and stabilize the mesoporous structures. Cooperation interaction mechanism can be considered as an acceptable model for the structural formation in the synthesis of mesoporous silica films.     

高岭石基介孔复合材料的二氧化碳吸附性能

碳排放量的快速增长所引起的全球气候变暖问题越来越受到各国的关注,因此研发制备可行高效的二氧化碳(CO₂)捕获材料具有极其重要的意义。本文以高岭石为原材料,采用煅烧-碱活化-酸刻蚀的方法,制备出介孔氧化硅载体(KNH),再将KNH经过五乙烯六胺(PEHA)修饰后制备出介孔复合材料(KNH-PEHA)。通过X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、N₂物理吸附等方法对样品进行表征,并进一步对样品进行CO₂吸附性能研究。结果表明,PEHA的浸渍修饰并未改变载体的结构,但显著提高了介孔复合材料对CO₂的吸附能力。吸附温度为25 ℃,KNH的CO₂吸附量为147.39 cm³/g,而PEHA质量分数为30%的KNH(KNH-P-30)平衡时的CO₂吸附量达到389 cm³/g,远高于未经PEHA修饰的KNH的吸附量,同时提出了该固体吸附剂对CO₂的吸附机理,为高岭石在气体吸附领域的应用提供一个新思路。     

沉积时间对Zn(O,S)薄膜性能及Cu2ZnSnSe4薄膜电池的影响

无镉材料Zn(O,S)因其带隙宽且可调节、无毒无害等优点被作为缓冲层材料重点研究,通过化学水浴法制备Zn(O,S)薄膜,研究了沉积时间的不同(20~35 min)对Zn(O,S)薄膜的成分、结构特性、光学性能及形貌的影响.通过XRD测试可知,水浴法制备的Zn(O,S)薄膜为非晶态.通过透反射谱测试可知,薄膜的光学透过率较高(>80;).通过表面形貌测试可知,30 min时Zn(O,S)薄膜为致密均匀的小颗粒.将Zn(O,S)薄膜应用在CZTSe电池中,在30 min时获得较高器件转换效率5.37;.     

Electron microscopy studies of epitaxial MgB2 superconducting thin films grown by in situ reactive evaporation

The morphology and chemistry of epitaxial MgB₂ thin films grown using reactive Mg evaporation on different substrates have been characterized by transmission electron microscopy methods. For polycrystalline alumina and sapphire substrates with different surface planes, an MgO transition layer was found at the interface region. No such layer was present for films grown on MgO and 4-H SiC substrates, and none of the MgB₂ films had any detectable oxygen incorporation nor MgO inclusions. High-resolution electron microscopy revealed that the growth orientation of the MgB₂ thin films was closely related to the substrate orientation and the nature of the intermediary layer. Electrical measurements showed that very low resistivities (several μΩ cm at 300 K) and high superconducting transition temperatures (38 to 40 K) could be achieved. The correlation of electrical properties with film microstructure is briefly discussed.     

雾化辅助化学气相沉积法氧化镓薄膜生长研究

采用自主设计搭建的雾化辅助化学气相沉积系统设备,开展了Ga₂O₃薄膜制备及其特性研究工作。通过X射线衍射研究了沉积温度、系统沉积压差对Ga₂O₃薄膜结晶质量的影响。结果表明,Ga₂O₃在425~650 ℃温度区间存在物相转换关系。随着沉积温度从425 ℃升高至650 ℃,薄膜结晶分别由非晶态、纯α-Ga₂O₃结晶状态向α-Ga₂O₃、β-Ga₂O₃两相混合结晶状态改变。通过原子力显微镜表征探究了生长温度对Ga₂O₃薄膜表面形貌的影响,从475 ℃升高至650 ℃时,薄膜表面粗糙度由26.8 nm下降至24.8 nm。同时,高分辨X射线衍射仪测试表明475 ℃、5 Pa压差条件下的α-Ga₂O₃薄膜样品半峰全宽仅为190.8″,为高度结晶态的单晶α-Ga₂O₃薄膜材料。     

Coordination of aluminum in amorphous sodium aluminosilicate films

Amorphous sodium aluminosilicate thin films containing large amounts of Al₂O₃ were deposited on fused silica substrates by rf-sputtering, and their aluminum K-band X-ray emission spectra were measured by using an electron probe X-ray microanalyser in order to determine the coordination number of aluminum ions in the amorphous thin films.

The chemical shifts for the amorphous films with Al₂O₃/Na₂O<1 were almost identical with those of tetrahedrally coordinated aluminum ions in microline. On the other hand, for the amorphous films with Al₂O₃/Na₂O>1, the chemical shifts increased with increasing Al₂O₃/NA₂OF ratio, approaching that of amorphous alumina. From the comparison with the chemical shifts of -Al₂O₃ and mullite, the coordination state of aluminum ions in amorphous alumina was found to be about 5, and its structure was found similar to be that in crystalline Al₂O₃ with spinel-type structure. These results indicate that in amorphous sodium aluminosilicate thin films aluminum ions exist in the tetrahedrally coordinated state when the Al₂O₃/Na₂O ratio is nearly equal to or less than unity. However, when the Al₂O₃/Na₂O ratio exceeds unity, some of the aluminum ions begin to assume the octahedrally coordinated state and increase in number with increasing Al₂O₃/Na₂O ratio.     

Crystallization behavior and hydrophilic performances of V2O5–TiO2 films prepared by sol–gel dip-coating

Homogeneous and transparent V₂O₅–TiO₂ composite nanometer thin films were prepared on glass substrates by sol–gel processing and dip-coating technique. The films as well as the dried powder of bulk gel were characterized by different techniques like X-ray diffraction (XRD), high-resolution scanning electron microscopy (HRSEM), atomic force microscope (AFM) and thermogravimetry–differential thermal analysis (TG–DTA). The hydrophilicity of the films was determined by measuring the water contact angles on the films. The results showed that the dopant of V₂O₅ on TiO₂ thin films could produce a visible-light response to the films, and the introduction of V₂O₅ could suppress the structural phase transition and crystal growth of TiO₂ crystal. Finally, the relationship between crystalline size and hydrophilicity under sunlight was investigated in this article.     

Electrosynthesis and characterization of [Cu(Taab)(H2O)2](L)2 non-crystalline thin films

Molecular-material thin films of diaqua tetrabenzo (b,f,j,n) {1,5,9,13} tetraazacyclohexadecine copper (II) bisanthraflavates and base organic molecules L have been electrodeposited on Corning 7059 glass slices, quartz substrates with tin oxide film and (100) single-crystalline silicon (c-Si) wafers. The surface morphology and structure of the deposited films were studied by atomic force microscopy (AFM), energy-dispersive spectrophotometry (EDS), ultraviolet-visible (UV-Vis) and Fourier-transform infrared (FT-IR) spectroscopies. The IR-spectra show that compounds obtained by chemical synthesis have the same absorption bands as the amorphous thin films obtained by electrosynthesis. The conductivities and the electrical-conduction mechanisms in the thin films were also investigated. Cubic nonlinear optical (NLO) characterizations of the film samples were performed with the Z-Scan technique, with some samples exhibiting remarkably high nonlinear activity.     

(111)取向0.7PMN-0.3PT薄膜机电耦合性能

铁电薄膜由于其优异物理性能,而被广泛应用于微电子、光电子、微机电领域。在铁电薄膜理论研究方面,热力学理论可以有效地预测铁电薄膜的相结构、极化特性和机电性能等,且已在(001)取向铁电薄膜的研究中取得了较好的应用,而对于(111)取向铁电薄膜的研究报道非常少。因此,本文通过对序参量坐标转换的方法,构建了(111)取向薄膜的热力学势能函数及其机电性能计算方法。基于此,研究了(111)取向0.7PMN-0.3PT铁电薄膜的相结构及其机电性能。研究结果表明,(111)取向0.7PMN-0.3PT铁电薄膜的相结构主要存在沿晶轴方向三个极化可互换的对称相:顺电相PE、菱方相R和单斜相M_A(或M_B)。在应变和外电场的调控下,(111)取向0.7PMN-0.3PT薄膜展现出优良的机电性能,在R和M_A相变点处,介电常数ε11、ε22、ε33和面外压电系数d33取得了极大值。在外电场E₃分别为0、50 kV/cm、100 kV/cm和200 kV/cm时,面外介电常数ε33的峰值分别为4 382、2 646、2 102和1 600,面外压电系数d33的峰值分别为303.8 pm/V、241.9 pm/V、219.7 pm/V和195.1 pm/V。应变和外电场能够较好地调控薄膜的机电耦合性能,可为优异机电耦合性能的器件制备提供参考。     

射频磁控溅射氧气流量对制备的Ga2O3∶Cr薄膜光致发光性能的影响

在不同氧气流量下,采用双靶射频磁控共溅射的方法在蓝宝石(α-Al₂O₃)基底上制备得到系列掺Cr的Ga₂O₃(Ga₂O₃∶Cr)薄膜,详细研究了薄膜在900 ℃退火前后的结构和光学性能。结果表明,未退火的Ga₂O₃∶Cr薄膜为非晶结构,其发光主要位于蓝绿波段。经900 ℃退火后,薄膜的结构由非晶变为多晶,且在近红外波段观测到了来源于Cr³⁺掺杂的发光。退火后的薄膜结晶质量和近红外发光均与氧气流量密切相关,而其光学带隙不受氧气流量的影响。在所研究的氧气流量范围,4 mL/min氧气流量下薄膜的近红外发光强度最强,这与此条件下薄膜结晶质量较好以及Cr³⁺替代Ga³⁺的数量较多有关。以上研究成果可为制备高质量Ga₂O₃∶Cr薄膜提供参考。     

沉积温度对电沉积PbS薄膜结构和性能的影响

采用电沉积法在ITO导电玻璃表面沉积了PbS薄膜,并用X射线衍射仪(XRD)、原子力显微镜(AFM)以及傅立叶变换红外光谱仪(FT-IR)对薄膜的结构和光学性能进行了表征,研究了沉积温度对薄膜的相组成、显微形貌以及光学性质的影响.结果表明:在U=3 V,pH=2.5,T=60 ℃,沉积时间为20 min,加入EDTA作络合剂的情况下,可制备出沿(111)和(200)晶面取向生长的立方相PbS薄膜.薄膜显微结构均匀而致密,随着反应温度从20 ℃增加到60 ℃,薄膜内的压应力逐渐减小,禁带宽度也随着变小.所制备的微晶PbS薄膜的禁带宽度约为0.39 eV.     

钴酸钙薄膜的制备及高温吸波性能研究

以溶胶凝胶法制备的钴酸钙粉体为基础材料,在氧化铝陶瓷基板上涂覆烧结形成了钴酸钙薄膜,研究了薄膜的物相结构、温阻特性及电磁波吸收性能。研究发现,溶胶凝胶法制备的钴酸钙粉体由Ca₉Co₁₂O₂₈相组成,粉体颗粒均匀,具有一定的取向性生长,呈明显的片层状结构。烧结后的钴酸钙薄膜由细小的Ca₃Co₄O₉相组成,与氧化铝基板结合紧密,厚度在20 μm左右,薄膜的方阻值随着温度的升高迅速下降,在300~800 ℃保持在20 Ω/□左右。800 ℃钴酸钙电阻膜型超材料吸波体在8~18 GHz显示出了对电磁波双吸收峰特征。     

Homoepitaxial growth of 6H–SiC thin films by metal-organic chemical vapor deposition using bis-trimethylsilylmethane precursor

Homoepitaxial silicon carbide (SiC) films were grown on 3.5° off-oriented (0 0 0 1) 6H–SiC by metal-organic chemical vapor deposition (MOCVD) using bis-trimethylsilylmethane (BTMSM, C₇H₂₀Si₂). A pronounced effect of the growth conditions such as source flow rate and growth temperature on the polytype formation and structural imperfection of the epilayer was observed. The growth behavior was explained by a step controlled epitaxy model. It was demonstrated by high-resolution X-ray diffractometry and transmission electron microscopy that high-quality 6H–SiC thin films were successfully grown at the optimized growth condition of substrate temperature 1440°C with the carrier gas flow rate of 10 sccm.     

氩气退火时间对Fe(Se,Te)薄膜的性能影响研究

作为一种铁基超导薄膜,Fe(Se,Te)薄膜具有晶体结构简单、所包含的元素较少、易于合成的特点,不仅有利于超导机理研究而且有着潜在的技术应用价值。本文通过磁控溅射在温度为320 ℃的CaF₂单晶衬底上制备了Fe(Se,Te)薄膜,并在氩气氛围下进行了退火处理。研究了退火时间对Fe(Se,Te)薄膜的晶体结构、微观形貌、成分组成以及电输运特性的影响。结果表明:Fe(Se,Te)薄膜的结晶性较好,退火有助于消除薄膜样品中的FeSe相,薄膜的晶格常数c对退火不敏感,退火后薄膜晶粒尺寸变大;Fe(Se,Te)薄膜成分与靶材的名义组分存在一定的偏差,退火时间越长,Fe(Se,Te)薄膜表面的颗粒越密集;Fe(Se,Te)薄膜的电阻随温度升高而减小,呈现出半导体特性,退火3 h后电阻明显增大。