氧化热处理对VO2薄膜特性的影响研究

采用直流磁控溅射法,结合氧化法热处理在硅基底上制备VO2薄膜,通过SEM、XRD、XPS、FTIR红外透射率等测试,从多角度分析了氧化热处理对VO2薄膜截面结构、晶相成分、成分价态、红外透射率相变特性的影响。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,氧化热处理有利于VO2晶粒生长并增加薄膜致密性,同时其红外透射率具有明显相变特性,相变温度为60.5 ℃,3~5 m、8~12 m波段的红外透射率对比值达到99.5%,实现了对红外波段辐射的开关功能,适合应用于红外探测器的激光防护研究,同时可为深入研究对薄膜的氧化热处理提供参考依据。     

氩氧比与退火温度对磁控溅射VO2薄膜结构与电学性能的影响

采用反应直流磁控溅射法,通过调控溅射过程中的氩氧比,在石英玻璃衬底上制备了氧化钒薄膜,研究了溅射气氛及后处理条件对其微结构与电学性能的影响.经450和500℃退火,薄膜中易形成VO2,而550℃退火时薄膜中会形成大量非4价的钒氧化物.薄膜在较高温度500℃下退火时结晶度增加,但薄膜颗粒之间的间隙更为明显,导致电阻率显著提高;同时其电阻率-温度曲线的热滞回线宽度较窄,在加热过程中相转变温度较高.当氩氧比中氧含量增加时,沉积的VO2薄膜中生成了少量非4价的钒氧化物.结果表明,反应磁控溅射法制备的氧化钒薄膜的微结构、电阻率、相变温度等特性与氩氧比和后退火温度密切相关.     

热处理时间对氧化钒薄膜相变性能的影响

采用直流磁控溅射的方法在普通玻璃上制备了低价的氧化钒薄膜,在氧气和氩气混合气氛中,对所制备的薄膜进行不同时间的热处理,得到具有相变特性的VO2薄膜。分别利用X射线衍射(XRD)和场发射扫描电镜(SEM)分析了薄膜的组分、结晶结构和表面形貌,利用四探针法测试了薄膜的电阻。结果表明:热处理前的氧化钒薄膜主要成分为V2O3,经过热氧化处理后,低价的氧化钒被氧化,薄膜中VO2含量增加,薄膜发生金属-半导体相变,其中450℃、2h为最佳处理参数,其电阻相变幅度超过2个数量级,薄膜的相变温度仅为30℃。     

VO2/FTO复合热致变色薄膜的制备及其光学特性

在掺氟的SnO2(FTO)导电玻璃衬底上采用直流磁控溅射的方法室温沉积纯钒金属薄膜,再在退火炉中经后退火工艺制备VO2/FTO复合热致变色薄膜,并对复合薄膜的结构及其光学特性进行研究.结果表明,导电玻璃上的FTO并没有改变VO2择优取向生长,但明显改变了VO2薄膜的表面形貌特征.与相同工艺条件下在玻璃衬底上制备的VO2薄膜相比,VO2/FTO复合薄膜的相变温度降低约18℃,热滞回线温宽收窄约4℃,相变前后的红外透过率分别约为42%和21%.说明复合薄膜既可明显降低相变温度和热滞宽度,又可增强VO2薄膜的红外调控能力.     

ZnSe基片上制备二氧化钒薄膜及退火改变组分研究

VO2作为相变材料在激光防护领域有着广阔的应用前景,为了提高透过率,采用在红外波段透过率为70%的ZnSe做基片,用磁控溅射法制备了VO2薄膜.对不同条件下制备的VO2薄膜用X射线电子能谱仪(XPS)测试,并通过拟合来得到VO,V2O3,VO2和V2O5在薄膜中所占的比例.为提高4价钒的含量对薄膜进行了退火处理,根据薄膜中的钒氧的比例,采用了充氧加热退火,退火时间4 h,退火温度450℃,退火真空度2.5×10-2Pa,氧气流量6.5 sccm.4价钒含量提高到了接近60%,分析了退火对氧化钒薄膜中4价钒含量的影响.     

磁控溅射氧化钒相变薄膜的电阻温度特性测量

利用MS500-B超高真空磁控溅射镀膜机,分别采用氧化法和还原法在普通玻璃基底上制备了二氧化钒(VO2)相变薄膜;并在20⁸0℃内往复变化时,利用XMT-100数字精密温度计和SX1934数字四探针测试仪测量两类样品的电阻-温度特性曲线。结果表明,两类样品均具有热敏相变特性;氧化法制备薄膜的电阻为9.9680℃内往复变化时,利用XMT-100数字精密温度计和SX1934数字四探针测试仪测量两类样品的电阻-温度特性曲线。结果表明,两类样品均具有热敏相变特性;氧化法制备薄膜的电阻为9.96⁰.06kΩ,相变温度约为30℃;还原法制备薄膜的电阻为80.30.06kΩ,相变温度约为30℃;还原法制备薄膜的电阻为80.3⁷.4kΩ,相变温度约为52℃。     

基于VO2/TiO2/FTO微结构的电压诱导相变存储器特性

相变存储器作为下一代具有竞争力的新型存储器,其基础和核心是相变存储介质.为了制备基于VO2薄膜的非易失性相变存储器,首先采用等离子体增强化学气相沉积法在氟掺杂二氧化锡(FTO)导电玻璃衬底上沉积一层厚度为100 nm的TiO2薄膜,再通过直流磁控溅射法制备VO2薄膜,并在TiOJFTO复合薄膜上形成VO2/TiO2/FTO微结构,用X射线衍射仪(XRD)、扫描电子显微镜(SEM)、四探针测试仪和半导体参数测试仪表征分析微结构的结晶和非易失性相变存储特性.结果表明,N2和O2的体积流量比为60∶40时,在TiO2/FTO上可生长出晶向为〈110〉的高质量VO2薄膜,在VO2/TiO2/FTO微结构两侧反复施加不同的脉冲电压,可观测到微结构具有非易失性相变存储特性,在67,68和69℃温度下的相变阈值电压分别为8.5,6.5和5.5V,相比多层膜结构的相变阈值电压降低了约37％.     

光诱导氧化钒薄膜原位太赫兹波调制特性研究

采用磁控溅射及快速热氧化法在c-Al2O3基底制备出高质量的氧化钒薄膜。首先,分析结果表明所制备的氧化钒薄膜表面颗粒大小均匀,表面均方根粗糙度约为16.75 nm,主要成分为VO2和V2O5,V4+离子的含量为78.59%,所制备的氧化钒薄膜具有稳定的热致相变特性;其次,光诱导下薄膜的THz波调制特性研究结果显示,随着激励光功率增大,薄膜的THz透过率逐渐减小;最后,经过多次原位反复测试结果表明所制备的氧化钒薄膜具有稳定可逆的THz波调制特性,可应用于太赫兹开关和调制器等集成式太赫兹功能器件。     

VO2-xNy薄膜的主要制备工艺参数与相变温度系数

选用V2O5为前驱物,通过在玻璃片上镀膜,利用高纯氢和高纯氮作为气源,采用微波等离子体增强法,在低温条件下合成了具有优良热致相变特性的氮杂二氧化钒(VO2-xNy)薄膜.通过正交试验设计对制备VO2薄膜过程中的主要影响因素(反应时间、反应压力、反应功率和N2/H2流量比)进行了分析研究.试验结果表明,VO2薄膜的最终的相变温度明显受到反应时间、反应压力、反应功率和N2/H2流量比的影响.其中以反应时间影响作用最为显著.经分析得到使VO2薄膜具有最低相变温度的优化工艺为:反应时间为7 min,反应压力为1.5 kPa,反应功率为100 W,N2/H2流量比为5/20(mL/min).文中对试验结果进行了简单讨论.     

VOx薄膜的制备、电阻-温度特性及结构研究

VO2是一种热致相变材料.发生相变时,VO2的电阻、红外光透过率、反射率都会发生显著变化.采用直流反应磁控溅射法,通过改变氧氩比(O2:Ar)、工作气压、衬底温度等制备工艺参数,研究了工艺参数对VOx薄膜的结构、电阻-温度性能的影响.结果表明,当氧氩比为1.0:15、工作气压为2.0Pa时,制备的薄膜中VO2的含量较多;衬底温度为250℃时,制备的VOx薄膜的电阻一温度突变性能最佳.     

Structural and Electrical Characters of Ba0.6Sr0.4TiO3/La0.5Sr0.5CoO3 Thin Films by Plus Laser Deposition

Epitaxial Ba0.6Sr0.4TiO3 (BST) thin films were deposited on LaAlO3 (LAO) substrates with the conductive metallic oxide La0.5Sr0.5CoO3 (LSCO) film as a bottom electrode by pulsed laser deposition (PLD). X-ray diffraction ~2 and Ф scan showed that the epitaxial relationship of BST/LSCO/LAO was [001] BST//[001] LSCO//[001] LAO. The atomic force microscope (AFM) revealed a smooth and crack-free surface of BST films on LSCO-coated LAO substrate with the average grain size of 120 nm and the RMS of 1.564 nm for BST films. Pt/BST/LSCO capacitor was fabricated to perform CapacitanceVoltage measurement indicating good insulating characteristics. For epitaxial BST film, the dielectric constant and dielectric loss were determined as 471 and 0.03, respectively. The tunabilty was 79.59% and the leakage current was 2.6310-7 A/cm2 under an applied filed of 200 kV/cm. Furthermore, it was found that epitaxial BST (60/40) films demonstrate well-behaved ferroelectric properties with the remnate polarization of 6.085 C/cm2 and the coercive field of 72 kV/cm. The different electric properties from bulk BST (60/40) materials with intrinsic paraelectric characteristic are attributed to the interface effects.     

Mg和V2O5共溅射制备+4价钒的氧化物薄膜

在常温、高真空条件下,采用高纯金属镁靶和V₂O₅靶进行共溅射,利用镁原子的还原性,将+5价的钒还原为+4价,在硅衬底上制备钒的氧化物薄膜。当Mg和V的原子比为1:2时,XPS测试表明薄膜中有V4+和V2+存在。X射线衍射结果显示,制备的薄膜主要成分是MgV₂O₅,且结晶状况良好。温度-电阻率测试结果显示,薄膜在20℃附近有相变行为,电阻温度系数高达－8.6%/K,回线弛豫温度约为0.3℃,负温度系数热敏电阻材料常数高达6700。这一发现为制备非制冷焦平面探测用的热敏薄膜材料提供了新的思路。     

Si衬底上具有Poly-Si/SiO2堆叠缓冲层的Pb (Zr0.52Ti0.48)O3 存储电容

在p型Si衬底上沉积多晶硅薄膜和Pb(Zr0.52Ti0.48)O3 (PZT)薄膜形成过渡层。测试淀积在多晶硅上的PZT薄膜不同退火温度的X射线衍射峰。Pt/PZT/poly-Si电容被研究。由于PZT薄膜的铁电极化特性,金属/铁电/多晶硅/二氧化硅/Si结构存储电容在650度退火展示了其顺时针的电压-电容曲线。存储窗口随着SiO2电容和PZT电容的耦合比的增加而增大。     

Electroluminescence from Au/Si/SiO2/p-Si structure

Si/SiO₂ films have been grown using the two-target alternation magnetron sputtering technique. The thickness of the SiO₂ layer in all the films was 8 nm and that of the Si layer in five types of the films ranged from 4 to 20 nm in steps of 4 nm. Visible electroluminescence (EL) has been observed from the Au/Si/SiO₂/p-Si structures at a forward bias of 5 V or larger. A broad band with one peak 650–660 nm appears in all the EL spectra of the structures. The effects of the thickness of the Si layer in the Si/SiO₂ films and of input electrical power on the EL spectra are studied systematically.     

非晶态SiO2过渡层对生长C轴取向LiNbO3薄膜的影响

采用磁控溅射方法,在Si衬底和LiNbO3薄膜之间引入SiO2过渡层制备LiNbO3薄膜。采用X射线衍射（XRD〉、傅里叶变换红外吸收光谱（FT-IR）和扫描电子显微镜（SEM）对LiNbO3薄膜的结晶取向、组成成分和表面形貌进行了表征,重点研究了非晶态SiO2过渡层对LiNbO3薄膜C轴取向的影响。结果表明,非晶态S...     

Effect of titanium dioxide (TiO2) seed layer on the phase composition of 0.7Pb (Mg1/3Nb2/3)O3-0.3PbTiO3 film prepared by pulsed laser deposition

Lead-magnesium niobate-lead titanate (PMN-PT) thin films with and without the TiO₂ seed layer were deposited on Pt/Ti/SiO₂/Si substrates through pulsed laser deposition. The study aimed to characterize the effect of the TiO₂ seed layer on the phase composition and properties of PMN-PT film. Without the TiO₂ seed layer, the pure perovskite phase could be obtained in the thinner PMN-PT film while with the TiO₂ seed layer, the pure perovskite phase was formed in the thicker PMN-PT film. The ferroelectric properties of PMN-PT films with the TiO₂ seed layer were exhibited. As a result, the maximum amount of remnant polarization reached the amount of 32 μC/cm² for the PMN-PT thin film with the TiO₂ seed layer.     

用溶胶-凝胶法制备的Cu2Bi2Cr2O8薄膜 及其光学和铁磁性能研究

以硝酸铜Cu(NO₃)₂·3H₂O、硝酸铬Cr(NO₃)₃·9H₂O、硝酸铋Bi(NO₃)₃·3H₂O和乙二醇为原料,利用溶胶-凝胶工艺在石英衬底上制备了纳米Cu₂Bi₂Cr₂O₈薄膜。通过X射线衍射(X-Ray Diffraction, XRD)和拉曼测试对样品进行了表征。结果表明,Cu₂Bi₂Cr₂O₈薄膜具有良好的光学特性,其禁带宽度为1.49 eV;在磁性测试方面,Cu₂Bi₂Cr₂O₈薄膜呈现出了良好的铁磁性。     

Etching characteristics and plasma-induced damage of Ba0.65Sr0.35TiO3 thin films etched in CF4/Ar/O2 plasma

Sol-gel-derived Ba_0.65Sr_0.35TiO₃ (BST) thin films were etched in CF₄/Ar/O₂ plasma using magnetically enhanced reactive ion etching technology. The maximum etch rate of BST film is 8.47 nm/min when CF₄/Ar/O₂ gas mixing ratio is equal to 9/36/5. X-ray photoelectron spectroscopy analysis indicates the accumulation of fluorine-containing by-products on the etched surface due to their poor volatility, resulting in (Ba,Sr)-rich and (Ti,O)-deficient etched surface. Compared to the unetched counterparts, the etched Ba 3d_5/2, Ba 3d_3/2, Sr 3d_5/2, Sr 3d_3/2, Ti 2p_3/2, Ti 2p_1/2 and O 1s photoelectron peaks shift towards higher binding energy regions by amounts of 1.31, 1.30, 0.60, 0.79, 0.09, 0.46 and 0.50 eV, respectively. X-ray diffraction (XRD) analysis reveals that intensities of the etched BST (1 0 0), (1 1 0), (2 0 0) and (2 1 1) peaks are lowered and broadened. Raman spectra confirm that the Raman peaks of the etched film shift towards lower wave number regions with the values of 7, 6, 4 and 4 cm⁻¹, and the corresponding phonon lifetimes are longer than those of the unetched film because of the plasma-induced damage. When the etched films are postannealed at 650 °C for 20 min under an O₂ ambience, the chemical shifts of Ba 3d, Sr 3d, Ti 2p and O 1s peaks, the variations for atomic concentrations of Ba, Sr, Ti and O, and the Raman redshifts are reduced, while the corresponding XRD peak intensities increase. It is conceivable that the plasma-induced damage of the etched film could be partially recovered during the postannealing process.     

Preparation of n-type semiconductor SnO2 thin films

We studied fluorine-doped tin oxide on a glass substrate at 350℃using an ultrasonic spray technique. Tin（Ⅱ） chloride dehydrate,ammonium fluoride dehydrate,ethanol and NaOH were used as the starting material, dopant source,solvent and stabilizer,respectively.The SnO₂:F thin films were deposited at 350℃and a pending time of 60 and 90 s.The as-grown films exhibit a hexagonal wurtzite structure and have（101） orientation.The G = 31.82 nm value of the grain size is attained from SnO₂:F film grown at 90 s,and the transmittance is greater than 80%in the visible region.The optical gap energy is found to measure 4.05 eV for the film prepared at 90 s, and the increase in the electrical conductivity of the film with the temperature of the sample is up to a maximum value of 265.58（Ω·cm）^-1,with the maximum activation energy value of the films being found to measure 22.85 meV,indicating that the films exhibit an n-type semiconducting nature.     

Electroluminescence of SrAl2O4:Eu phosphor

The SrAl₂O₄:Eu²⁺ phosphor powders have been synthesized by sol-gel process. Electroluminescent (EL) properties of the SrAl₂O₄:Eu²⁺ phosphor were investigated using a convenient thick film device. Green light emitting at a peak of 508 nm was obtained when driven by sine alternating current (AC). The color coordinate of the emission was x=0.148 and y=0.635. Luminance-voltage and afterglow characteristics of the SrAl₂O₄:Eu²⁺ EL devices were studied. The results show that SrAl₂O₄:Eu²⁺ can be used as green phosphor for EL displays.