电结晶铜/钴纳米多层膜结构与磁性能研究

以n型Si(111)为基底, 在硼酸镀液体系中采用双槽法电结晶制备Cu/Co纳米多层膜, 确定了工艺条件. 用扫描电镜(SEM)和X射线衍射(XRD)对纳米多层膜的结构和形貌进行了表征, 显示多层膜具有良好周期性和超晶格结构. 并用物性测量系统PPMS测试了不同结构 Cu/Co纳米多层膜的磁性能. 磁滞回线表明: 不同周期数的纳米多层膜其矫顽力均较小. 巨磁阻(GMR)性能与纳米多层膜结构有关. GMR值随Co磁性层厚度增长先增大后减小, 有一极值; 随着Cu非磁性层厚度的增加GMR值发生周期性的振荡; 随周期数N的增大, GMR值先增大, 在N为60时达到了90%, 随着N的继续增加而减小, 当达到80周期时, GMR值趋于稳定.     

自旋阀多层膜的电化学制备及其巨磁电阻效应

采用双槽控电位电沉积法在n-Si(111)基体上以NiFe 薄膜为缓冲层制备了[Ni80Fe20/Cu/Co/Cu]n自旋阀多层膜, 并确定了电沉积的工艺条件. 利用X射线衍射(XRD)表征了自旋阀多层膜的超晶格结构, 研究了NiFe缓冲层对自旋阀生长取向的影响. 采用四探针法研究了各子层厚度对自旋阀巨磁电阻效应的影响, 通过振动样品磁强计(VSM)测试了自旋阀的磁滞回线. 自旋阀的巨磁电阻(GMR)值最初随着铜层厚度的变化并发生周期性振荡, Cu 层厚度为3.6 nm时, GMR 达到最大值,随后逐渐减小. 随着Co层和NiFe 层厚度的增大, GMR 值的变化趋势均为先增大后减小. 当自旋阀的结构为NiFe(25 nm)/[Cu(3.6 nm)/Co(1.2 nm)/Cu(3.6 nm)/NiFe(2.8 nm)]30时, GMR 值可达5.4%, 对应的磁电阻灵敏度(SV)为0.2%·Oe-1, 饱和磁场仅为350 Oe.     

热处理对[NiFe/Cu/Co/Cu]_n多层纳米线磁性能的影响

采用双槽控电位法在阳极氧化铝(AAO)模板中制备了有序均一的[NiFe/Cu/Co/Cu]n多层纳米线阵列,并在不同温度下进行了热处理.利用X射线衍射(XRD)对热处理前后多层线的晶体结构进行了测试.考察了不同退火温度对多层线矫顽力、剩磁比、巨磁电阻(GMR)效应、磁灵敏度的影响.随热处理温度升高,多层纳米线中磁性微晶晶型取向越来越明显,晶体结构更均匀;多层纳米线的矫顽力和剩磁比先增大后减小.300°C下多层纳米线矫顽力达到最大值,GMR最大值可达59%,对应的磁电阻灵敏度(SV)为0.233%Oe-1.     

超晶格多层膜的电化学制备、表征及其GMR特性的研究

以半导体Si为衬底,电化学沉积Cu/Co超晶格多层膜,用SEM表征多层膜的断面形貌.XRD研究表明,多层膜的调制波长为20～160 nm时,膜层间发生外延生长.随着调制波长的减小,外延生长对膜层结构的影响越来越明显.当调制波长小于20 nm时,在XRD强衍射峰的两侧出现卫星峰,表明多层膜形成超晶格结构.根据卫星峰位置计算的调制波长与由法拉第定律估算的结果非常接近.多层膜的巨磁电阻(GMR)性能随多层膜周期数的增加而增大;当周期数大于300时,GMR性能基本上不再随周期数变化,说明基体的导电性质对GMR的影响可以忽略.     

小周期金属多层膜厚度评价

超晶格多层膜是随着现代科技的进步而发展起来的新一代电子薄膜材料,半导体超晶格和量子阱多层膜材料在光电子领域已经占据了不可取代的地位。1988年,法国科学家在由Fe、Cr交替沉积而形成的[Fe/Cr]金属多层膜中发现了超过50%的磁电阻变化率,这种现象被称为巨磁阻效应(GMR)[1]。     

纳米金属多层膜与多层纳米线的电化学制备及其表征

分别采用单槽法和双槽法电沉积Cu/Co多层膜.研究了两种电沉积方法制备多层膜的工艺条件,利用电化学方法、XRD和SEM对多层膜进行表征,并对Cu/Co多层膜的巨磁阻性能进行了测试. 采用电沉积多层膜的方法，以多孔铝阳极氧化膜（AAO）为模板,在纳米孔内沉积Cu/Co多层线,采用TEM对多层纳米线进行了表征.     

退火温度对CdSe纳米薄膜的形成及光电性能影响

在室温下,采用循环伏安法在ITO上沉积CdSe纳米薄膜。利用X射线衍射仪(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(AFM)、X射线光电子能谱分析(XPS)、紫外-可见(UV-VIS)分光光度计以及电化学工作站对不同温度退火后的CdSe纳米薄膜的晶体结构、形貌、光学性能、光电化学性能进行表征和测试。结果表明,退火温度对CdSe纳米薄膜的形貌和性能起到关键性作用。薄膜表面平整、厚度均匀,且由呈纳米颗粒状的立方相CdSe构成;经退火后,CdSe纳米颗粒出现不同程度的长大现象,Se含量随退火温度的升高而减少。紫外-可见吸收光谱表明随着退火温度的升高,CdSe纳米薄膜对可见光的吸收发生红移,表明禁带宽度逐渐减小,表现出量子尺寸效应。通过光电流测试表明随着退火温度的升高,CdSe薄膜的光电响应效应显著提高。     

退火温度对CdSe纳米薄膜的形成及光电性能影响

在室温下,采用循环伏安法在ITO上沉积CdSe纳米薄膜。利用X射线衍射仪(XRD)、场发射扫描电镜(FESEM)、原子力显微镜(AFM)、X射线光电子能谱分析(XPS)、紫外-可见(UV-VIS)分光光度计以及电化学工作站对不同温度退火后的CdSe纳米薄膜的晶体结构、形貌、光学性能、光电化学性能进行表征和测试。结果表明,退火温度对CdSe纳米薄膜的形貌和性能起到关键性作用。薄膜表面平整、厚度均匀,且由呈纳米颗粒状的立方相CdSe构成;经退火后,CdSe纳米颗粒出现不同程度的长大现象,Se含量随退火温度的升高而减少。紫外-可见吸收光谱表明随着退火温度的升高,CdSe纳米薄膜对可见光的吸收发生红移,表明禁带宽度逐渐减小,表现出量子尺寸效应。通过光电流测试表明随着退火温度的升高,CdSe薄膜的光电响应效应显著提高。     

Fe/RE多层膜磁性及其变化机制

研究了Ｆｅ／ＲＥ多层膜（Ｆｅ单层厚度〈２．０ｎｍ）沉积态退火过程中（温度≥４７３Ｋ）的结构与磁性，分析了磁性变化的原因。沉积态的Ｆｅ单层由分离的Ｆｅ岛组成，小尺寸的Ｆｅ岛呈超顺磁性导致了整个膜显示顺磁性，退火时Ｆｅ岛合并长大，膜由超顺磁转变为铁磁，同时磁化强度和妖顽力增加。     

退火处理对LaFeO3/Pd复合薄膜微观结构和在碱液中电化学行为的影响

采用射频磁控溅射装置在Si(111)衬底上分别制备了Pd单膜、LaFeO3单膜和LaFeO3/Pd复合薄膜,利用XRD,SEM,EDS,XPS和电化学测试方法研究了退火处理对LaFeO3/Pd薄膜材料的相结构、形貌、化学组成以及电化学性能的影响。研究结果表明:未退火的溅态LaFeO3薄膜呈无序非晶态结构,随退火温度升高,600℃退火1 h后LaFeO3薄膜晶化为钙钛矿型正交结构,此时薄膜晶粒尺寸呈增大趋势;800℃退火时,随退火时间增加,薄膜晶粒尺寸变化不明显,退火前LaFeO3薄膜表面平整、致密,退火后薄膜表面出现裂纹。XPS分析表明,LaFeO3薄膜中的氧以晶格氧、化学吸附氧和物理吸附氧三种结合状态形式存在,退火后LaFeO3薄膜中化学吸附氧转变为晶格氧。电化学测试结果表明,Pd膜电极和LaFeO3膜电极放电容量很低(3.9~19 mAh·g-1),而LaFeO3/Pd复合薄膜在退火前后的电极放电容量分别达到50和180.7 mAh·g-1,LaFeO3单膜和LaFeO3/Pd复合薄膜电极的交换电流密度I0分别为为3.36和590.51 mA·g-1。镀Pd后能极大改善和提高LaFeO3/Pd复合膜电极的电催化活性和电化学放电容量。     

Systematic study on structural phase behavior of CdSe thin films

Cadmium selenide (CdSe) thin films were chemically deposited at room temperature, from aqueous ammoniacal solution using Cd(CH(3)COO)(2) as Cd2+ and Na(2)SeSO(3) as Se2- ion sources. The as-deposited films were uniform, well adherent to the glass substrate, specularly reflective, and red-orange in color. The as-deposited CdSe layers grew with nanocrystalline sphalerite cubic structure along with the amorphous phase present in it, with optical band gap E(g) = 2.3 eV. The films were annealed in air atmosphere for 4 h at different temperatures and characterized for compositional, structural, morphological, and optical properties. XRD and SEM studies clearly revealed the systematic phase transformation of CdSe films from metastable nanocrystalline cubic (zinc blende type) to a mixture of cubic and hexagonal (wurtzite type), and finally into stable hexagonal through different intermediate phases with an improvement in the crystal quality. The films showed a red shift in their optical spectra after annealing.     

In situ Raman spectroscopy of H2 interaction with WO3 films

It is well known that WO(3) interacts efficiently with H(2) gas in the presence of noble metals (such as Pd, Pt and Au) at elevated temperatures, changing its optical behaviors; and that its crystallinity plays an important role in these interactions. For the first time, we investigated the in situ Raman spectra changes of WO(3) films of different crystal phases, while incorporating Pd catalysts, at elevated temperatures in the presence of H(2). The Pd/WO(3) films were prepared using RF sputtering and subsequently annealed at 300, 400 and 500 °C in air in order to alter the dominant crystal phase. The films were then characterized using SEM, XRD, XPS, and both UV-VIS and Raman spectroscopy. In order to fundamentally study the process, the measurements were conducted when films were interacting with 1% H(2) in synthetic air at elevated sample temperatures (20, 60, 100 and 140 °C). We suggest that the changes of Raman spectra under such conditions to be mainly a function of the crystal phase, transforming from monoclinic to a mix phase of monoclinic and orthorhombic achieved via increasing the annealing temperature. The as-deposited sample consistently shows similar Raman spectra responses at different operating conditions upon H(2) exposure. However, increasing the annealing temperature to 500 °C tunes the optimum H(2) response operating temperature to 60 °C.     

Structural, morphological, and magnetic study of nanocrystalline cobalt-nickel-copper particles

Nanocrystalline Co(x)Ni(y)Cu(100-x-y) particles were synthesized by the reduction of metal acetates in a mixture of polyol and Tween 80. Inductively coupled plasma (ICP) analysis revealed that the actual wt% of Co, Ni, and Cu in these nanoparticles was nearly the same as in the starting solutions. The structures of the particles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area electron diffraction (SAED) spectroscopy, and vibrating sample magnetometry (VSM). The results of XRD and VSM confirmed that there was no metastable alloying in the particles. The particles were composites, consisting of nanoscale crystallites of face-centered cubic (fcc) Cu, face-centered cubic (fcc) Ni, and face-centered cubic (fcc) Co. During preparation the nucleation of Cu occurred first; then small Cu nuclei acted as cores for the precipitation of Co and Ni. The particles showed an increase in saturation magnetization (M(s)) as the concentration of Co or Ni in the particles was increased. The changes of both M(s) and coercivity of the particles with increasing annealing temperatures were studied. The coercivity of the particles was very high; it could reach as high as 489 Oe for Co34.3Ni31.2Cu34.5) .     

Structure and morphology of nanostructured zinc oxide thin films Prepared by dip-vs. spin-coating methods

In this study, we use dipping and spinning methods to coat glass slides with sol-gel ZnO thin films, composed of zinc acetate dihydrate, monoethanolamine (MEA), de-ionized water and isopropanol. The effect of the annealing temperature on the structural morphology and optical properties of these films is investigated. These ZnO films were preheated at 275 °C for 10 min and annealed either at 350, 450 or 550 °C for 60 min. As-deposited films, formed by amorphous zinc oxide-acetate submicron particles, are transformed into a highly-oriented ZnO after thermal treatment. The surface morphology, phase structure and optical properties of the thin films were investigated by scanning electron microscopy, X-ray diffraction (XRD) and optical transmittance. Both techniques produced nanostructured ZnO thin films with well-defined orientation. The annealed films were transparent in the visible range with an absorption edge at about 375 nm and a transmittance of ca 85–90% with an average diameter of 40 nm. XRD results show the film was composed of polycrystalline wurtzite, with a preferential c-axis orientation of (002) and a single sharp XRD peak at 34.40, corresponding to the hexagonal ZnO. The grain size is increased by the annealing temperature. Both coating techniques create sol-gel ZnO films with the potential for application as transparent electrodes in optic and electronic devices.     

电沉积Co-Cu颗粒膜的巨磁电阻效应

从１９８８年Ｂａｉｂｉｃｈ首先在磁性Ｆｅ／Ｃｒ多层膜中发现巨磁电阻效应（ＧＭＲ）以来 ［１］,由于ＧＭＲ本身的科研价值和在磁记录、磁性传感器等方面的广泛应用前景 ,引起了人们的极大关注．继多层膜之后 ,人们在金属颗粒膜如Ｃｏ Ａｇ［２］,Ｃｏ Ｃｕ［３,４］等中也相继发现了巨磁电阻效应．颗粒膜是微颗粒镶嵌于薄膜中所构成的复合材料体系．原则上 ,颗粒的组成与薄膜的组成在制备条件上应互不固溶 ,因此颗粒膜区别于合金、化合物 ,属于非均匀相组成的材料．磁性颗粒膜是磁性粒子分布在非磁性金属材料薄膜中．在磁性颗粒与非…     

低温熔盐中电沉积Sm-Co合金膜及其磁性能

在353 K的尿素-乙酰胺-NaBr-KBr熔体中, 用恒电位电解法在Cu基片上制备了Sm-Co合金膜. 利用循环伏安法研究了熔体的电化学行为. 电化学实验结果表明, 在Pt电极上, Co(II)+2e→Co(0)是一步完全的不可逆反应; 测得CoCl2-尿素-乙酰胺-NaBr-KBr熔体中, Co(II)在Pt电极上的传递系数α=0.31, 扩散系数D0=4.78×10^-5 cm2·s-1; Sm(III)难以单独沉积, 但能被Co(II)诱导共沉积, 在不同阴极电位下制备出不同Sm含量的非晶合金膜. 用等离子发射光谱仪(ICP)检测薄膜成分, 用SEM观察了薄膜的表面形貌结构, 用XRD和振动样品磁强计(VSM)分析样品退火前后的晶相和磁性能变化特征. 结果表明, 在923 K进行退火30 s后Sm-Co薄膜由非晶转变为多晶结构, 并以hcp晶相结构为主; 退火和Sm含量对Sm-Co合金膜的磁性能有重要的影响.     

Controlling the growth of particle size and size distribution of silica nanoparticles by the thin film structure

Nanostructured silicondioxide thin films were prepared by sol–gel spin coating technique. The SiO₂ films were made using a conventional mixture of tetraethoxysilane (TEOS), deionized water and ethanol with various NH₃/TEOS ratios. The nanostructured silica films were made using a mixture of the SiO₂ sol and regular SiO₂ sol to control the enlargement of the particles inside the films. The structural, morphological and optical characterizations of the as-deposited and annealed films were carried out using X-ray diffraction (XRD), atomic force microscopy, scanning electron microscopy, NKD spectrophotometer and ultraviolet–visible (UV–vis) spectroscopy. The transmittance data of the infrared spectra of the films were recorded using an FT-IR Spectrometer. The XRD studies showed that as-deposited films were amorphous and the formation of the alfa-cristobalite phase of the silica film was investigated at annealing temperature close to 1,100 °C. Optical properties of the transmittance spectra in the s and p-polarization modes were collected. Refractive indices and extinction coefficients were determined with respect to the NH₃/TEOS ratios in the compositions of the films. Optical cut-off wavelength values were investigated from the extrapolation of the absorbance spectra which was estimated from the UV–vis spectroscopy measurements. A red shift in the absorption threshold indicated that the size of silica nanoparticles was increased by an increase in the NH₃/TEOS volume ratio from 1:64 to 1:8.     

脉冲激光沉积LiFePO4阴极薄膜材料及其电化学性能

采用脉冲激光沉积结合高温退火的方法在不锈钢基片上制备了LiFePO₄薄膜电极. XRD谱图显示, 经650 ℃退火制得的是具有橄榄石结构的LiFePO₄薄膜. 充放电测试表明, LiFePO₄薄膜具有3.45/3.40 V的充放电平台, 与LiFePO₄粉体材料相当. 首次放电容量约为27 mAh•g^－1, 充放电循环100次后容量衰减51%.     

耐蚀Zn-Al合金材料的组合材料芯片方法优选

应用组合材料芯片方法, 通过离子束溅射法制备了全组分范围的Zn-Al薄膜样品阵列. 沉积得到的多层薄膜经370 ℃扩散处理2 h形成合金薄膜. 通过扫描俄歇能谱仪(AES)、X射线衍射仪(XRD)及扫描电子显微镜(SEM)对样品的成分、结构和形貌进行表征. 结果显示, 在低温退火后, 合金薄膜成分均匀, 结晶良好, 表面致密. 材料芯片上的样品在0.1 mol·L-1氯化钠溶液中的极化电阻测试结果表明, 对于全组分的Zn-Al合金薄膜, Al摩尔分数在87%附近的成分具有最高的极化电阻值.进一步的实验发现, 在83%-86%这一较宽的摩尔分数区间内, 极化电阻值均保持在105 Ω·cm-2以上, 比传统热镀锌镀层的极化电阻高1个数量级.     

Phase transition properties of vanadium oxide films deposited by polymer-assisted deposition

Vanadium dioxide (VO₂) films were synthesized on mica substrates by a polymer-assisted deposition method, followed by rapid annealing with different annealing temperatures. The crystalline structure and morphology of the films were investigated by XRD and FE-SEM, and their phase transition properties were studied by in situ FT-IR. The results indicated that the annealing temperature affected the crystalline structure and morphology of the films remarkably, which then resulted in varied phase transition properties. In particular, the films annealed at higher temperature showed more polycrystalline structure, increased particle size and reduced phase transition intensity. But the films exhibited the similar hysteresis temperature width with increasing annealing temperature.