低温热氧化处理温度与时间对氧化钒薄膜性能的影响

采用直流对靶磁控溅射氧化钒薄膜再附加热氧化处理的方式进行金属-半导体相变特性氧化钒薄膜的制备,研究了低热处理温度下热处理温度与时间对氧化钒薄膜组分、晶体结构和相变性能的影响.新制备的氧化钒薄膜为V2O3和VO的混合相.经300℃/1h热处理后,薄膜内出现单斜结构VO2,薄膜具有相变特性;保持热处理时间不变,升高热处理温度至360℃,薄膜表面变得致密,致密的薄膜表面阻碍了氧气与薄膜内部V2O3和VO的反应,VO2成分含量与300℃/1h处理时的含量接近;增加热处理温度并延长热处理时间,如热处理条件为320℃/3h时,薄膜内VO2成分大量增多,电阻值变化幅度超过两个数量级;在300～360℃的热处理温度区间内,薄膜内V2O3和VO不断向VO2转变,相变性能变好,但对VO2的单斜金红石结构没有影响.     

氧化法热处理温度对氧化钒薄膜热敏特性的影响

采用直流磁控溅射法制备氧化钒薄膜,并采用不同的温度对其进行氧化法热处理,通过XRD、SEM、四探针薄膜电阻测试,分析了不同热处理温度对氧化钒薄膜的晶相特性与热敏特性的影响。实验分析证明热处理温度升高后(400℃)得到的薄膜热敏特性良好,其室温电阻为160KΩ·cm,室温电阻温度变化系数为-2.4%/℃,变温过程中(20~98℃)其平均值约-1.98%/℃,表明温度升高有利于改善薄膜热敏特性,在非制冷红外探测器应用方面具有发展潜力。     

溶胶凝胶法制备VO2薄膜的组织与性能研究

采用V2O5熔体淬水制成胶体，并浸涂于不同的基片上，分别用于电阻检测和组织结构分析。经过真空加热分解V2O5凝胶薄膜，得到了具有相变特性的VO2薄膜。在真空热处理温度为500℃，时间为34h，真空气压为2Pa，得到的VO2相变薄膜电阻突变量级达3.4，相变温度在67℃左右。另外，TEM组织观察表明，VO2薄膜为多晶组织，VO2薄膜晶粒尺寸对电阻突变量级影响较大。晶粒尺寸增加，电阻突变量级增大。VO2晶界对相变有阻碍作用。     

Ag衬底层对FePt薄膜结构和性能的影响

采用磁控溅射方法在自然氧化的单晶Si(100)衬底上制备了双层结构的FePt-X/Ag(X=Ag或Pt)薄膜.以20nm厚的Ag做衬底,可以制备出易磁化轴垂直基片的FePt合金薄膜;Ag在FePt薄膜中优先团聚,不利于控制FePt晶粒的长大,调整Pt的含量可以控制热处理过程中FePt薄膜的晶粒尺度;通过XRD、TEM、VSM对薄膜样品的结构、晶粒尺寸的观察和磁性检测,我们认为FePt合金薄膜有序化转变的最佳热处理温度在400℃;经过500℃热处理,薄膜软硬磁耦合较好,晶粒尺寸约为100nm,有最大的矫顽力1.04×106A/m.     

热处理对STO铁电薄膜微结构的影响

系统研究了 CFA与 RTA两种热处理方式以及热处理温度和时间对 STO 薄膜微结构的影响。STO薄膜采用脉冲激光沉积法(PLD)制备。采用原子力显微镜(AFM)和XRD分别对薄膜的表面形貌和晶粒结构进行分析。结果表明,在热处理温度 650~800℃范围内,相对于 CFA、STO薄膜经 RTA热处理后,薄膜表面晶粒大小分布均匀、致密。两种热处理方法都使薄膜的晶粒直径随温度升高而增大,并且温度越高,薄膜的晶形越完整,同样热处理温度下,RTA与CFA相比薄膜的晶粒较小, 两种热处理方法的最大晶粒尺寸都<120nm。但XRD分析结果表明,在相同热处理温度下,CFA 热处理的结晶转化率较 RTA 热处理要高。在一定范围内,RTA热处理时间对薄膜晶粒尺寸影响不大,热处理时间越长,晶粒更加完整,表面更加均匀平整,结晶转化率越高。     

磁控溅射制备VO_2薄膜及其红外相变特性

采用直流磁控溅射法与氧化法热处理相结合的工艺,在Si基底上制备VO2薄膜,通过扫描电镜(SEM)、X射线衍射(XRD)、X射线电子能谱(XPS)、傅里叶变换红外光谱(FTIR)透射率测试,分析了VO2薄膜截面结构、晶相成分、成分价态及红外透射率相变特性。实验分析表明,采用直流磁控溅射与氧化热处理相结合的方法,可获得主要成分为具有明显择优取向单斜金红石结构VO2(011)晶体的氧化钒薄膜,其红外透射率具有明显相变特性,相变中心温度为57.5℃,3~5μm、8~12μm波段的红外透射率对比值达到99.5%,适合应用于红外探测器的激光防护研究。     

纳米结构FePt薄膜的结构与磁性研究

采用磁控溅射方法在自然氧化的单晶Si（100）衬底上制备了纳米结构的Fe,Pt100-x（X=30at％-60at％）薄膜。高温XRD分析表明,薄膜在500℃热处理有明显的面心立方FCC结构向面心四方FCT结构转变。通过VSM、AFM对薄膜样品的磁性检测和晶粒尺度的观察,FePt合金薄膜有序化转变的最佳热处理温度在400—500℃,在这个热处理温度范围内,薄膜软硬磁耦合较好,矫顽力适当（306kA／m）,晶粒尺寸约为10nm,适合于做高密度磁记录介质材料。     

磁控溅射工艺对二氧化钒薄膜生长及场致相变性能的影响

为揭示VO2薄膜场致相变规律,指导氧化钒工业化规模制造与应用,使用磁控溅射直流溅射工艺在蓝宝石衬底上制备了VO2薄膜。对薄膜进行了XRD及SEM测试,分析了溅射氧分压、溅射温度及溅射压强对晶体组份、晶粒的生长趋势及晶体表面结构的影响规律。对VOx薄膜的场致相变特性进行了测试研究,分析了VOx薄膜的导电开关特性,总结了溅射氧氩比对其临界相变电场区间及电导率变化倍数的影响规律。得出结论,基片温度对成膜速度和晶粒大小及晶粒间隙有很大影响,溅射气压对薄膜表面晶体生长的均匀性影响显著,氧分压是影响薄膜组份的重要因素,氧氩比会影响薄膜的场致相变电导率变化倍数和临界相变电压区间。     

氧化钒薄膜的微观结构研究

采用直流反应磁控溅射法在不同基片上制备了80nm和1000nm厚的氧化钒薄膜.采用X射线衍射仪、原子力显微镜及扫描电镜进行了薄膜微观结构分析.结果表明,薄膜的晶化受衬底影响较大,晶化随膜厚的增加而增强.不同衬底上生长的薄膜晶粒尺寸存在较大差异,Si3N4/Si衬底上生长的薄膜晶粒细小,薄膜较为平坦;玻璃衬底、Si衬底和α-Al2O3陶瓷衬底上生长的薄膜晶粒较为粗大.随着膜厚的增加,薄膜的晶粒尺寸明显增大,不同衬底上生长的二氧化钒薄膜晶粒都具有一种独特的"纺锤"形或"棒"形.     

热处理对溶胶-凝胶TiO2薄膜的晶相转变和性能影响

以钛酸丁酯（TPOT）为有机醇盐前驱体，采用溶胶－凝胶技术制备了TiO2溶胶。为测量方便起见，分别制备了凝胶粉体和薄膜，并对样品进行了不同温度的热处理。X射线衍射（XRD）、椭偏仪和紫外－可见光谱（UV－vis)的测量表明：随热处理温度的升高，TiO2的结构由非晶到锐钛矿再到金红石相转变，400℃为锐钛矿相，600℃开始出现金红石相，800℃完全转变为金红石相；晶粒尺寸随热处理温度的升高而逐渐增大，锐钛矿结构的晶粒尺寸范围是2.5-5.5nm，金红石结构的晶粒尺寸范围是5.9-6.8nm；TiO2薄膜的折射率随热处理温度的升高而增大，同时薄膜厚度降低；禁带宽度随热处理温度的升高而增大，同时薄膜厚度降低；禁带宽度随热处理温度升高而变窄，锐钛矿结构的禁带宽度为3.45eV，而金红石结构的禁带宽度为3.30eV。     

氧化钒薄膜在玻璃基片上的生长研究

采用直流反应磁控溅射法, 在平整光滑的普通玻璃基片表面沉积了厚度分别为80nm、440nm和1μm的氧化钒薄膜. 采用原子力显微镜(AFM)、扫描电镜(SEM)和X射线衍射仪(XRD)对薄膜的表面形貌、结构和结晶化的分析表明, 厚度影响着薄膜的颗粒大小和结晶状态, 随着薄膜厚度的增加, 薄膜的颗粒增大, 晶化增强; 薄膜具有明显的垂直于衬底表面的“柱”状择优生长特征. 对薄膜的方阻和方阻随温度的变化进行了相关分析, 证实了厚度对氧化钒薄膜的电学性能存在明显的影响, 随着薄膜厚度的增加, 薄膜的方阻减小, 方阻温度系数升高, 薄膜的方阻随温度变化的回线滞宽逐渐增大, 薄膜的金属-半导体相变逐渐趋于明显.     

Nano-polycrystalline vanadium oxide thin films prepared by pulsed laser deposition

Nano-polycrystalline vanadium oxide thin films have been successfully produced by pulsed laser deposition on Si(100) substrates using a pure vanadium target in an oxygen atmosphere. The vanadium oxide thin film is amorphous when deposited at relatively low substrate temperature (500 degrees C) and enhancing substrate temperature (600-800 degrees C) appears to be efficient in crystallizing VOx thin films. Nano-polycrystalline V3O7 thin film has been achieved when deposited at oxygen pressure of 8 Pa and substrate temperature of 600 degrees C. Nano-polycrystalline VO2 thin films with a preferred (011) orientation have been obtained when deposited at oxygen pressure of 0.8 Pa and substrate temperatures of 600-800 degrees C. The vanadium oxide thin films deposited at high oxygen pressure (8 Pa) reveal a mix-valence of V5+ and V4+, while the VOx thin films deposited at low oxygen pressure (0.8 Pa) display a valence of V4+. The nano-polycrystalline vanadium oxide thin films prepared by pulsed laser deposition have smooth surface with high qualities of mean crystallite size ranging from 30 to 230 nm and Ra ranging from 1.5 to 22.2 nm. Relative low substrate temperature and oxygen pressure are benifit to aquire nano-polycrystalline VOx thin films with small grain size and low surface roughness.     

Barium titanate thin films deposited by electrophoresis on p-Doped Si (001) substrates

Barium titanate (BaTiO3) thin films have been prepared by electrophoretic deposition on p-doped and platinum covered silicon (Si) substrates. Their structure, nanostructure and dielectric properties were characterized. The as-deposited films were polycrystalline and composed by barium titanate nanograins with an average grain size approximately 9 nm. Annealing at high temperatures promoted grain growth, so that the samples annealed at 600 degrees C presented average grain sizes approximately 24 nm. From Raman spectroscopy measurements it was found that the tetragonal (ferroelectric) BaTiO3 phase was stabilized on the films. Also, at higher annealing temperatures, cation disorder was reduced on the films. From measurements of the temperature dependence of the dielectric permittivity the corresponding paraelectric-ferroelectric phase transition was determined. The observed transition temperature (approximately 100 degrees C) was found to be below the BaTiO3 bulk or thick film values, due to the small nanosized grains composing the films.     

掠射角溅射沉积纳米结构氧化钨薄膜

采用掠射角反应磁控溅射法在室温下沉积了纳米结构氧化钨(WO₃)薄膜, 并对薄膜进行热处理。利用场发射扫描电镜(FE-SEM)和X射线衍射仪(XRD)对氧化钨薄膜的形貌和结构进行了表征。当掠射角度为80°时, 采用直流电源沉积的氧化钨薄膜具有纳米斜柱状结构, 而采用脉冲直流电源沉积的薄膜呈现纳米孔结构。纳米薄膜经450℃热处理3 h后, 纳米斜柱彼此连接, 失去规整结构, 而纳米孔结构的孔尺寸变大。XRD分析表明室温沉积的氧化钨薄膜具有无定形结构, 经450℃热处理1 h后, 转变为单斜晶相。具有纳米斜柱状或纳米孔结构氧化钨薄膜的光学调制幅度在波长600 nm时达到60%, 且电致变色性能可逆。     

Structural and electrical properties of RuO2 thin films prepared by rf-magnetron sputtering and annealing at different temperatures

Conductive ruthenium oxide (RuO₂) thin films have been deposited at different substrate temperatures on various substrates by radio-frequency (rf) magnetron sputtering and were later annealed at different temperatures. The thickness of the films ranges from 50 to 700 nm. Films deposited at higher temperatures show larger grain size (about 140 nm) with (200) preferred orientation. Films deposited at lower substrate temperature have smaller grains (about 55 nm) with (110) preferred orientation. The electrical resistivity decreases slightly with increasing film thickness but is more influenced by the deposition and annealing temperature. Maximum resistivity is 861 μΩ cm, observed for films deposited at room temperature on glass substrates. Minimum resistivity is 40 μΩ cm observed for a thin film (50 nm) deposited at 540°C on a quartz substrate. Micro-Raman investigations indicate that strain-free well-crystallized thin films are deposited on oxidized Si substrates.     

Work function of vanadium dioxide thin films across the metal-insulator transition and the role of surface nonstoichiometry

Vanadium dioxide (VO(2)) undergoes a sharp metal-insulator transition (MIT) in the vicinity of room temperature and there is great interest in exploiting this effect in novel electronic and photonic devices. We have measured the work function of vanadium dioxide thin films across the phase transition using variable temperature Kelvin force microscopy (KFM). The work function is estimated to be ～5.15 eV in the insulating phase and increases by ～0.15 eV across the MIT. We further show that the work function change upon the phase transition is highly sensitive to near-surface stoichiometry studied by X-ray photoelectron spectroscopy. This change in work function is distinct from bulk resistance-versus temperature trends commonly used to evaluate synthesis protocols for such vanadium oxide films and optimize stoichiometry. The results are pertinent to understanding fundamental electronic properties of vanadium oxide as well as charge injection phenomena in solid-state devices incorporating complex oxides containing multivalence cations.     

[101]取向Li掺杂ZnO薄膜光学性能的研究

采用射频磁控溅射法在玻璃衬底上制备了[101]取向的Li:ZnO薄膜, 研究了该薄膜的光学性能随热处理温度变化的规律. 结果表明, 399nm的发光峰是由Li的杂质能级引起; 与[002]取向的薄膜相比, 未经热处理的[101]薄膜其光学带隙大, 且出现了380nm附近的带边发射(NBE) 峰; 在560～580℃热处理下, 其晶胞变小、光学带隙变窄、360nm 左右的带间发光峰红移; 当热处理温度升至610℃时, 薄膜中再次出现380nm的NBE峰.     

石英衬底上柱状多晶硅薄膜的制备

利用射频等离子体增强化学气相沉积法(RF-PECVD)在已经预沉积有非晶硅薄膜的石英衬底上低温沉积了N/I非晶硅薄膜, 对样品进行了两步快速光热(RTP)退火. 采用 Raman、X射线衍射(XRD)、扫描电子显微镜(SEM)和透射电子显微镜(TEM)等测试仪器对样品退火前后的结晶状况和微观形貌进行了分析. 结果表明, 该N/I非晶硅薄膜退火后的晶化率达到了94%左右, 断面形貌为柱状结构, 样品中的平均晶粒尺寸约30nm, 晶粒团簇的尺寸最大约1.5μm.     

Sol-gel法制备多铁性Bi_(0.85)Eu_(0.15)FeO_3薄膜及其性能

采用Sol-gel法在Pt/Ti/SiO2/Si衬底上制备了Bi0.85Eu0.15FeO3薄膜。研究了退火温度对其晶相形成的影响,发现在较低温度退火(450℃)时,Bi0.85Eu0.15FeO3晶相开始形成,但存在杂相,而且结晶度较差;在490～600℃可以获得结晶较好的单相Bi0.85Eu0.15FeO3薄膜。同时对经550℃退火的薄膜的介电、铁电和铁磁性能进行了研究,结果表明,Bi0.85Eu0.15FeO3薄膜具有较好的介电及铁磁性能。当测试频率为1MHz时,薄膜的介电常数和介电损耗分别为80、0.024,饱和磁化强度约为26.2emu/cm3。     

Characteristics of CeOx–VO2 composite thin films synthesized by sol–gel process

Pure vanadium dioxide (VO₂) and CeOx–VO₂ (1.5 < x < 2) composite thin films were grown on muscovite substrate by inorganic sol–gel process using vanadium pentaoxide and cerium(III) nitrate hexahydrate powder as precursor. The crystalline structure, morphology and phase transition properties of the thin films were systematically investigated by X-ray diffraction, Raman, X-ray photoelectron spectroscopy, FE-SEM and optical transmission measurements. High quality of the VO₂ and CeOx–VO₂ composite films were obtained, in which the relative fractions of +4 valence state vanadium were above 70 % though the concentrations of cerium reached 9.77 at %. However, much of cerium compounds were formed at the edge of grains and the addition of cerium resulted in more clearly defined grain boundaries as shown in SEM images. Meanwhile, the composite films exhibited excellent phase transition properties and the infrared transmittance decreased from about 70 to 10 % at λ = 4 μm bellow and above the metal–insulator phase transition temperature. The metal–insulator phase transition temperatures were quite similar with about 66 °C of the pure VO₂ and CeOx–VO₂ composite thin films. But hysteresis widths increased with more addition of cerium, due to the limiting effect of grain boundaries on the propagation of the phase transition. Particularly, the CeOx–VO₂ composite film with an addition of 7.82 at % Ce showed a largest hysteresis width with about 20.6 °C. In addition, the thermochromic performance of visible transmittance did not change obviously with more addition of cerium.