硫化压力对电沉积并硫化合成的FeS2薄膜组织结构的影响

采用电沉积及400℃不同压力硫化热处理制备了多晶FeS2薄膜,研究了硫化压力对薄膜晶体结构及微观组织的影响。在较低的硫化压力条件下,电沉积得到的Fe3O4先驱体硫化反应不充分,薄膜组织中FeS2与Fe3O4共存。当硫化压力高于20kPa时,Fe3O4先驱体可充分地转变成具有细小晶粒形态的FeS2,薄膜形貌也由多孔疏松演变为均匀平整。硫化压力在5～40kPa范围内变化对FeS2晶粒尺寸影响不明显,但使FeS2晶格常数略有下降。     

硫化时间对电沉积制备FeS2薄膜组织与结构的影响

利用电沉积及热硫化法制备了FeS2 多晶薄膜,研究了不同硫化时间对FeS2 薄膜形成过程的影响。结果表明采用Na2S2O3 和FeSO4 水溶液电沉积和150~ 200℃处理可以制备多孔Fe3O4 薄膜,再经400℃、80kPa硫化处理,Fe3O4 可转变成FeS2 多晶薄膜。随硫化时间延长到10h,FeS2 的晶格常数减小而晶粒粗化,再继续延长硫化时间,FeS2 的晶格常数增大而晶粒尺寸下降。可以用点缺陷浓度、相变应力及亚晶界运动等因素分析Fe3O4 向FeS2 转变过程中的微观组织参数变化规律。     

晶粒尺寸对FeS2薄膜微应变及光吸收特性的影响

采用不同厚度的Fe膜在673K热硫化20h制备出具有不同晶粒尺寸的FeS2薄膜，分析并测定了薄膜组织结构、微应变及光吸收性能．结果表明，Fe膜硫化形成的FeS2薄膜厚度在120—550nm范围内变化时，可导致平均晶粒尺寸在40-80nm之间变化．FeS2晶粒尺寸的变化造成了晶体面缺陷密度的变化，可引起微观内应力水平、缺陷能级分布和晶界势垒高度的变化，进而使得薄膜的微应变、点阵畸变度、光吸收系数及禁带宽度等物理特性随晶粒尺寸的增加而降低．     

薄膜生长基底对FeS2晶体取向的影响

用Fe膜硫化法制备了FeS2薄膜,分析了基底对FeS2薄膜晶体结构和位向分布的影响.结果表明,改变基底晶体的类型能够在一定程度上控制FeS2薄膜的晶体位向分布.FeS2薄膜在Si(100)、Si(111)和Al基底上可获得(200)方向的择优取向,在TiO2基底上可同时获得(200)及(220)择优取向,非晶玻璃基底对位向分布影响不明显.不同的基底与Fe薄膜的界面错配度不同,可改变薄膜晶体位向的分布,导致晶格畸变程度和晶粒尺寸的变化.当基底为非晶结构或界面的错配度较大时,FeS2晶体的取向分布主要受表面能和晶粒优先生长方向的控制,薄膜具有较小的晶格畸变和较细的晶粒;当基底为晶态并且界面错配度较小时,FeS2晶体取向的分布除受表面能及晶粒优先生长方向控制外,还受界面应变能的控制,此时薄膜易形成较大的晶格畸变和粗晶粒.     

晶体面缺陷对FeS2薄膜电学性能的影响

采用Fe膜热硫化技术制备了具有不同比表面积和比晶界面积的FeS2薄膜,并测定其载流子浓度和电阻率,研究了FeS2薄膜表面和晶界等面缺陷对FeS2薄膜电学性能的影响.结果表明,表面和晶界两种面缺陷对FeS2薄膜的电学性能有类似的影响规律.在一定范围内,随着薄膜比表面积和比晶界面积的增大,载流子浓度提高而电阻率下降.面缺陷数量的变化可导致FeS2晶体中点缺陷数量、禁带中缺陷能级密度、不充分相变产物比例和相变应力水平的变化,从而导致载流子浓度和电阻率的变化.     

粉末FeS2的合成及结构精修

实验采用Fe2O3粉末与纯铁粉末分别在100kPa硫压、恒温50h的条件下合成了FeS2粉体，并利用Rietveld方法对X射线衍射数据进行精修。结果表明在同样的条件下Fe2O3比铁粉更易与S结合生成FeS2，而且样品晶粒度明显增大。晶粒生长较好。     

Ni—Zn—Fe氢氧化物的低温自发固相反应

摩尔比为Ni2＋：Zn2＋：Fe3＋：0．6：0．4：2．0的水溶液与OH-在气泡液膜中进行共沉淀反应,制得0．6Ni（OH）2（H2O）0.75·（0．4-n）Zn（On）2·2（1-m—n）Fe（OH）3·mFezO3·nZnFe2O4·xH2O前驱体,微结构为大量螺旋状分子簇和少量亚晶结构,用XRD检测结果表明,前驱体在室温放置10和14个月的转化产物是Fe2O3,ZnFe2O4和Nin6Znn．Fe2O4;放置55个月的主要产物是Nin6Znn4Fe2O4。提出了分子簇演绎氢氧化物脱水,优先生成Fe2O3晶核,亚晶结构演绎新生态氧化物分子自组装的低温自发固相反应机理。     

SnO2共混Fe2O3纳米氧化物的制备及其组织结构研究

用SnCl4和FeCl3为原料,采用化学共沉淀法制备掺杂Fe2O3的纳米SnO2,运用差热(DSC)、X射线粉末衍射(XRD)和透射显微镜(TEM)等方法对Fe2O3和SnO2混杂纳米粉末的物相和粒径进行了分析。结果发现：与纯SnO2相比,(1)掺杂Fe2O3可以降低前驱体Sn(OH)4分解制备SnO2纳米晶的焙烧温度,从纯Sn(OH)4的分解温度345．7℃下降到341．1℃;(2)掺杂Fe2O3可以有效阻碍SnO2纳米晶的团聚和长大,前驱体在650℃焙烧时,纯SnO2晶粒在25nm,而掺杂Fe2O3的SnO2晶粒可以保持在2nm左右;(3)掺杂Fe2O3使前驱体焙烧制备SnO2的温度范围更宽,对制备小于10nm的SnO2纳米晶,纯SnO2的焙烧温度范围在400～550℃,而掺杂Fe2O3的焙烧温度范围在400～650℃;(4)SnO2／Fe2O3复合粉末在650℃以下,其晶体结构保持溶剂SnO2的四方结构,部分Fe元素置换了Sn的位置;650℃以上,复合粉末从溶剂晶格中析出Fe2O3形成两相结构。     

微弧氧化法制备磁性薄膜的研究

采用微弧氧化法以FeSO4溶液在钛金属表面制备超顺磁性薄膜．用IR、XRD和SEM等表征了磁性薄膜的组成和形貌，结果表明磁性薄膜主要由Fe3O4和（Fe2O3）x·2H2O晶体组成．推断了磁性薄膜的形成机理．     

Al/MoO3和Al/Fe2O3纳米含能薄膜制备与性能表征

使用自动控制磁控溅射仪制备纳米级Al/MoO3和Al/Fe2O3含能薄膜,使用扫描电镜(SEM)、原子力显微镜(AFM)对其形貌进行分析,使用X射线衍射(XRD)、X射线光电子能谱(XPS)分析薄膜组分,利用差示扫描量热(DSC)进行热力学分析。分析显示,含能薄膜结构完整,层状结构清晰;Al/MoO3纳米薄膜中MoO3有较大部分被还原为Mo2O5和MoO2,Al/Fe2O3纳米薄膜中Fe2O3有部分被还原为FeO,含能薄膜中Al有少部分被氧化为非晶结构的Al2O3。含能薄膜放热峰起始温度较低,活化能较小,反应活性较高,放热量较大,分别为3198和1680J/g。     

Sulfurization time effects on the growth of Cu2ZnSnS4 thin films by solution method

Cu₂ZnSnS₄ (CZTS) films were obtained by sulfurizing (Cu, Sn) S/ZnS structured precursors prepared by a combination of the successive ionic layer absorption and reaction method and the chemical bath deposition method, respectively. The effect of sulfurization time on structure, composition and optical properties of these CZTS thin films was studied. The results of energy dispersive spectroscopy indicate that the annealed CZTS thin films are of Cu-poor and Zn-rich states. The X-ray diffraction studies reveal that Cu_2?x S phase exists in the annealed CZTS thin film prepared by sulfurization for 20 min, while the Raman spectroscopy analysis shows that there is a small Cu₂SnS₃ phase existing in those by sulfurization for 20 and 40 min. The band gap (E _g ) of the annealed CZTS thin films, which are determined by reflection spectroscopy, varies from 1.49 to 1.56 eV depending on sulfurization time. The best CZTS thin film is the one prepared by sulfurization for 80 min, exhibiting a single kesterite structure, dense morphology, ideal band gap (E _g  = 1.55 eV) and high optical absorption coefficient (>10⁴ cm^?1).     

The surface free energy of pyrite films prepared by sulfurizing the precursive electrodeposited films

The pyrite films were prepared by sulfurizing the precursive films at different temperatures. The microstructure, chemical compositions and surface free energy have been investigated. The results indicate that pyrite films are obtained after the sulfuration process of precursive films. The sulfuration temperature remarkably influences the contact angle. Using Owens and Wendt geometric mean approach, the surface free energy, the dispersive surface free energy and polar surface free energy can be evaluated based on the value of contact angles. It has been found that the surface free energy is significantly dependent on the sulfuration temperature and chemical compositions of films. With the increase of the sulfuration temperature, the dispersive surface free energy decreases but the polar surface free energy keeps basically invariable. A possible relationship between the surface free energy and film quality has been discussed.     

Preparation of Fe3O4 Film by in-situ Oxidative Hydrolysis on Chitosan

The Fe3O4 films were prepared by in-situ oxidative hydrolysis on chitosan. The structures and characteristics of the prepared Fe3O4 films were investigated by X-ray diffractometry （XRD）, scanning electron microscopy （SEM）, atom force microscopy （AFM）, vibrating sample magnetometry （VSM） and thermogravimetric-differentia thermal analysis （TG-DTA）. The results show that, （1） the as-synthesized Fe3O4 films are pure Fe3O4 with cubic inverse spinel structure; （2） the network structured film can be obtained at lower temperature, and the compact particle film at higher temperature; （3） the prepared Fe3O4 films are super-paramagnetic, and the saturation magnetization is improved with increasing the reaction temperature, which is 49.03 emu/g at 80℃; （4） the temperature of phase transformation from Fe3O4 to a-Fe2O3 is about 495℃. Besides, the formation mechanism of Fe3O4 film was also proposed.     

Synthesis of type-II textured tungsten disulfide thin films with bismuth interfacial layer as a texture promoter

Highly textured tungsten disulfide (WS₂) thin films have been obtained by sulfurization of tungsten trioxide. The properties of WS₂ thin films prepared with bismuth interfacial layer as texture promoter has been studied. The WS₂ thin films were found to have predominant type-II orientation. The stacking of 2H-WS₂ crystallites observed with scanning electron microscopy was not reported hitherto. The films can be pictured as an assembly of WS₂ hexagonal crystallites. The energy dispersive X-ray analysis and X-ray photoelectron spectroscopy (XPS) studies confirm that the films are stoichiometric. The XPS analysis described the local environment of the tungsten atoms and the formal oxidation states of the tungsten and sulfur atoms were + 4 and − 2. Together with the high degree of crystallinity and excellent texture of the film, a relatively smooth morphology, on submicron scale, is revealed through atomic force microscopy study. The conditions for the desired textured growth with the van der Waals planes parallel to the substrate surface are reported.     

Microstructure and optical absorption of FeS2 films formed by sulfurizing precursive iron of various crystallite scales

Precursive iron films with various crystallite scales were prepared by sputtering on substrates heated at different temperatures. The iron films were annealed in sulfur vapor at 673 K to form pyrite films. The structural and optical characters were determined. High substrate temperatures produce large crystallites in the precursive iron films. The pyrite films are composed of a surface layer with coarse columnar grains and a bottom layer with fine equiaxed grains. Sufficient formation and growth of iron grains result in improved crystallinity of the pyrite films. The optical absorption characteristics depend mainly on the crystallinity of the pyrite films or the crystallizing status of the precursive iron films. The optical absorption coefficient of the pyrite films decreases with the increase of iron grain diameter from 12 to 39 nm. The band gap of the pyrite films increases with the increase of iron grain diameter from 12 to 53 nm.     

Pyrite (FeS2) thin films deposited by sol-gel method

Nanocrystalline pyrite (FeS₂) films were achieved by the sol-gel dip-coating process and sulfurization treatment. The microstructural, optical and electrical characteristics were investigated and the effect of sulfurization time on film properties was discussed. The XRD spectra show that FeS₂ film can be obtained for 1 h sulfurization and no other phase appears. The morphology of the precursor Fe₂O₃ films shows a porous and loose structure. However, with the sulfurization time increasing, the precursor films completely transformed into the pyrite films which have a compact and smooth structure. The pyrite films with a different sulfurization time have the optical absorption edges changed in the range of 0.90-0.99 eV. With the increase of sulfurization time, the carrier concentration increases and the carrier mobility decreases. It is speculated that crystallographic defects in the films could play an important role in film properties.     

FeS2/TiO2复合薄膜光电性能

采用溶液浸渍法在ITO导电玻璃表面的多孔TiO2薄膜上沉积了FeS2薄膜.使用Fe2O3粉末保护裸露在外的ITO导电膜在硫气氛中热处理后,制得了FeS2/TiO2复合薄膜.应用B531/H数显测厚指示表、数字式四探针测试仪、XJCM-8太阳电池测试仪等研究了FeS2/TiO2复合薄膜的厚度、ITO导电玻璃的电阻率以及FeS2/TiO2复合薄膜的光电性能.结果表明：此方法制得的FeS2/TiO2复合薄膜具有良好的光电性能;且ITO导电膜的电阻率变化较小.因而适宜制备色素增感太阳能电池（DSSC）.     

Green synthesis of uniform magnetite (Fe3O4) nanoparticles and micron cubes

Single-crystalline Fe3O4 microcubes were obtained through a green hydrothermal procedure using Fe3+, Fe2+ and H2O2 as starting materials. The structures and morphologies of the as-prepared samples were characterized in detail by X-ray diffraction (XRD), Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) respectively. Magnetite (Fe3O4) cubes averaging 3 microm in diameter were synthesized by H2O2 oxidation of Fe3+ and Fe2+ under neutral conditions. The contrastive experiments were designed to elucidate the effects of Fe3+, Fe2+ and H2O2 on the morphology of the final products. Irregular and ellipsoidal Fe2O3 structures were obtained by H2O2 oxidation of Fe3+ and Fe2+ respectively. Meanwhile, Fe3O4 nanotubes and nanoparticles were obtained when H2O2 was replaced by NH4HCO3 and urea respectively. The results show that H2O2, Fe3+ and Fe2+ in the reactive system play critical roles in obtaining micrometric cube-like Fe3O4. While, other nanometric Fe2O3 and Fe3O4 particles with tube-like and other morphologies could also be developed by controlling the reaction parameters.