XPS结合氩离子溅射剖析Si/C多层膜的化学状态

采用X射线光电子能谱结合氩离子溅射对用作锂离子电池负极的Si/C多层膜进行了表面测试及深度剖析,获得了Si/C多层膜结构中不同深度位置的成分及化学状态.分析结果表明,Si/C多层膜中各层Si、C薄膜之间存在界面元素相互扩散,扩散至相邻层薄膜中的Si、C元素主要以化合物SiC形式存在,且处于不同位置的SiC的化学键能受周...     

Si片上PbTiO3薄膜的XPS研究

用溶胶 凝胶方法在Si上成功地制备了钙钛矿型的PbTiO3薄膜。X射线衍射结果显示 ,在热处理温度为 750～ 90 0℃范围内 ,随温度升高 ,薄膜由多晶结构转变为定向结晶。X射线光电子能谱分析发现 ,薄膜表面存在SiO2 薄层 ,其厚度大约为 0 6nm ,该薄层是在制膜过程中衬底Si通过PbTiO3薄膜扩散到表面与大气中的O2 反应而形成的。在 750℃热处理的薄膜 ,膜层中不含SiO2 ,但温度升高 ,膜层中存在SiO2 成分 ,这可能是Si在向表面扩散过程中与膜中的O反应生成的。表面SiO2 可通过Ar离子的轻微溅射而消除 ,而膜内SiO2 成分只能通过调节工艺参数来消除     

氧离子束辅助激光淀积生长ZnO/Si的研究

利用X射线衍射(XRD),X射线摇摆曲线(XRC)和X射线光电子能谱(XPS)分析方法对氧离子束辅助激光淀积生长的ZnO/Si异质结薄膜进行了分析.结果表明:用该法可生长出高度c轴单一取向ZnO薄膜,XRC的半高宽度(FWHM)仅为2.918°.表明此生长方法经优化,可生长出单晶质量很好的ZnO/Si薄膜.     

热氧化对Zr基块体金属玻璃腐蚀行为的影响

本文系统研究了空气中热氧化对Zr-Cu-(Nb)-Ag-Al-Be块体金属玻璃在含Cl~-溶液中腐蚀行为的影响。热氧化后:样品表面生成0.3~0.4μm厚的氧化层,层内Al和O富集;含Nb样品点蚀电位和自然腐蚀电位明显增大,不含Nb样品极化曲线却无明显变化;浸泡实验中样品表面的腐蚀坑密度显著降低,腐蚀坑内Cu富集、Zr贫化。X射线光电子能谱结果显示热氧化后含Nb样品表面含有Nb_2O_5和更低的Cu含量,而其它元素与不含Nb样品相似。因此,热氧化能更显著地改善含Nb样品耐蚀性能的原因可能是含Nb_2O_5的氧化膜更加致密,以及该氧化层能更有效阻碍Cl~-扩散。     

纳米SiC表面接枝修饰的XPS研究

聚合物在纳米粒子表面接枝后,可在其表面建立起空间位阻稳定层,提高纳米粒子的分散稳定性及其与树脂基体的相容性.本文采用缩聚法在纳米SiC表面接枝了聚缩醛,X射线光电子能谱(XPS)的分析结果表明,经过聚缩醛接枝改性的纳米SiC表面Si2p峰明显降低,而C1s峰和O1s峰明显地增长,对C1s、Si2p峰精细扫描及分峰拟合表明,纳米SiC表面碳元素中有38.4%属于接枝物聚缩醛的有机碳,而79.8%的Si元素结合能增加了2.5eV,由此表明,纳米SiC表面形成了良好的表面修饰层,接枝物聚缩醛以化学键结合于纳米SiC表面;对比XPS和热失重分析(TG)的数据结果,可以推测,聚缩醛主要分布在纳米SiC的表面,而在体相中独立存在的几率较小.     

硅掺杂辉光放电聚合物薄膜的成分结构分析

以H2、反式二丁烯(T2B)和四甲基硅烷(TMS)混合气体为工作气体,在不同TMS流量条件下,用低压等离子体增强化学气相沉积法制备了Si掺杂辉光放电聚合物(GDP)薄膜。采用傅里叶变换红外光谱表征了不同TMS流量下Si掺杂GDP薄膜的化学组成结构。X射线光电子能谱表征了Si掺杂GDP薄膜成分,分析了TMS流量对Si掺杂GDP薄膜化学结构与元素组成的影响。研究表明:薄膜中成功地掺入了Si元素;Si掺杂GDP薄膜中Si元素主要以Si-C,Si-H等键合形式存在;在TMS流量为0.5~2 mL/min(标准状态)的范围内,薄膜中Si的原子浓度为0.72%~1.35%;随着TMS流量的逐渐增加,薄膜中Si含量逐渐增大。     

不同衬底温度下生长的Bi1.5Zn1.0Nb1.5O7.0薄膜的XPS研究

采用固相反应法合成具有焦绿石立方结构的Bi1.5Zn1.0Nb1.5 O7(BZN)陶瓷靶材,采用脉冲激光沉积法在Pt/TiO2/SiO2/Si(100)基片制备立方BZN薄膜,衬底温度在500～ 700℃范围内变化.X射线衍射测量结果表明:当在500℃沉积BZN薄膜时,薄膜呈现出无定形态结构.随着衬底温度增加到550℃,薄膜开始晶化,并且显示出立方焦绿石结构.X射线光电子能谱也被用来研究BZN薄膜的结构状态和元素价态.测试得到的全谱表明:在BZN薄膜中,除了用于定标的C元素之外,只有Bi、Zn、Nb、O元素的特征峰,此外有Ti2p特征峰出现,可能来自底电极的TiO2缓冲层.各元素的窄谱扫描表明:Bi,Zn,Nb,O四种元素的化学价态分别是+3,+2,+5,-2.BZN薄膜在550℃结晶,随着衬底温度升高到600℃,金属阳离子的结合能的峰位向高能方向移动,然而O1s的特征峰位也向高能方向移动,这归因于薄膜中存在的氧空位.     

PLD生长的ZnO薄膜的微结构及其发光特性研究

在不同的衬底温度下，通过脉冲激光淀积（PLD）方法在Si衬底上生长出c轴高度取向的ZnO薄膜。ZnO薄膜的结构分别通过X射线衍射（XRD）和广延X射线吸收精细结构（EXAFS）来表征，而表面成份和化学态则通过X射线光电子能谱来研究。利用光致发光（PL）来研究样品的发光特性。XRD结果和EXAFS结果都表明了500℃时生长的ZnO薄膜的结晶性比300℃时生长的要好。EXAFS结果和XPS结果显示，300℃时生长的ZnO薄膜处于富氧状态，而500℃时生长的则处于缺氧状态。结合XRD谱、EXAFS谱、XPS谱和PL谱的结果可以看到：随着ZnO薄膜的结晶性变好，它的紫外发光增强；另一方面，随着ZnO薄膜中O的含量减少，绿光发射变强。我们的结果表明绿光发射与ZnO中氧空位（V0）有关。     

硅基GaN外延层的SIMS及XPS研究

采用真空反应法在硅基上制备出了GaN外延层。利用二次离子质谱和X射线光电子能谱对GaN外延层进行了深度剖析和表面分析。结果表明 ,外延层中Ga和N分布均匀 ;在表面处Ga发生了偏聚 ;外延层中还存在Si,O等杂质 ,但这些并未影响到GaN外延层的物相及发光性能。实验还表明 ,在外延生长前采用原位清洗可去除Si衬底表面的氧     

非晶壳层SixN/SiyC包覆硅量子点的微结构表征

通过磁控溅射技术和1100℃的高温后退火处理,在富硅碳化硅薄膜中形成高密度小尺寸的硅量子点,硅量子点的结构由X射线光电子能谱和高分辨透射电镜进行表征,结果表明,在高温退火过程中,碳化硅薄膜发生了相分离,硅和碳的化学结合态在热力学的驱动下形成稳定的Si-Si键和Si-C键,同时,氮原子钝化了分解过程中形成的Si悬挂键,在硅量子点的表面形成SixN/SiyC非晶壳层。这种非晶壳层包覆量子点的结构配置非常有利于形成稳定的超小硅量子点 （1-3 nm）,此结构的量子效应所产生的光吸收了从绿光到紫外光的光谱范围,大幅度提高光伏太阳能电池的光电转换效率。     

Study of (Zr,Ti)CN, (Zr,Hf)CN and (Zr,Nb)CN films prepared by reactive magnetron sputtering

(Zr,Ti)CN, (Zr,Hf)CN and (Zr,Nb)CN coatings, in which Ti, Hf and Nb were added to ZrCN base compound, have been prepared by reactive magnetron sputtering. The coatings, with two different non-metal/metal ratios, were comparatively investigated in terms of elemental and phase composition, texture, surface morphology, hardness and friction performance. It has been shown that the films exhibit nanocomposite structures, consisting of a mixture of crystalline metal carbonitride and amorphous carbon. As compared with ternary ZrCN coatings, the quaternary coatings were found to exhibit superior mechanical and friction characteristics. In general, the films with higher non-metal content revealed finer morphologies, higher hardness and lower friction coefficient. Depending on the coating type and non-metal/metal ratio, the hardness values ranged from about 21 to 29 GPa, being higher than those of ZrCN reference films. The coefficients of friction varied from 0.2 to 0.5, the lowest values being obtained for the coatings with the highest non-metal content.     

单晶PMnN-PZT铁电薄膜制备与表征

利用磁控溅射方法,在MgO基底上沉积三元系铁电薄膜6%PMnN-94%PZT(6%Pb(Mn1/3,Nb2/3)O3-94%Pb(Zr0.45,Ti0.55)O3),采用淬火方法对薄膜进行后期热处理。分别运用面内和面外X射线衍射(XRD)技术分析薄膜长相及晶体结构,运用高分辨率扫描电镜(SEM)观察薄膜的晶粒表面及截面结构。实验结果表明,所沉积薄膜为单晶钙钛矿结构薄膜,薄膜结构优良。     

Mg/Nb复合薄膜的结构调控及其对脱氢温度的影响

利用磁控溅射法制备了两组Mg/Nb复合薄膜,研究了不同Nb层厚度和不同基底温度对Mg/Nb复合薄膜脱氢温度的影响。结果表明,当Nb层厚度为1nm和2nm时,其催化效果相对最好,可使Mg/Nb复合薄膜的脱氢温度分别降至110℃和122℃。当基底温度为125℃时对脱氢性能的改善效果最佳,可使Mg(100nm)/Nb(1nm)复合薄膜的脱氢温度降至100℃。同时,讨论了Nb层厚度和基底温度对Mg/Nb复合薄膜脱氢温度的影响机制。     

Reactive pulsed-DC sputtered Nb-doped VO2 coatings for smart thermochromic windows with active solar control

Thermochromic VO2 thin films have successfully been grown on SiO2-coated float glass by reactive pulsed-DC magnetron sputtering. Different Nb doping amounts were introduced in the VO2 solid solution during the film growing which resulted in films with distinct semiconducting-metal phase transition temperatures. Pure VO2 showed improved thermochromic behavior as compared with VO2 films prepared by conventional DC sputtering. The transition temperatures were linearly decreased from 59 down to 34 degrees C with the increase in Nb content. However, the luminous transmittance and the infrared modulation efficiency were markedly affected. The surface morphology of the films was examined by scanning electron microscopy (SEM) and showed a tendency for grain sized reduction due to Nb addition. Moreover, the films were found to be very dense with no columnar microstructure. Structural analyses carried out by X-ray diffractometry (XRD) revealed that Nb introduces significant amount of defects in the crystal lattice which clearly degrade the optical properties.     

(Zr,Al)N薄膜的微结构及性能研究

采用射频磁控反应溅射在单晶Si(100)上沉积了一系列不同Al含量的(Zr,Al)N薄膜,利用能谱仪(EDS)、X射线衍射仪(XRD)、扫描电镜(SEM)和微力学探针对薄膜的成分、结构、力学和抗氧化性能进行了表征。研究结果表明,当Al含量在0%~20.31%(原子分数)之间时,薄膜是B1型(NaCl)单相结构;当Al含量为31.82%时,同时出现B1和B4型(ZnS)双相结构。当Al含量超过36.82%时,以B4结构为主。随着铝含量的增加,薄膜晶面间距减小,晶格常数变小。薄膜的力学性能测试表明,适当的Al含量可以提高薄膜的硬度。随着Al含量的增加,薄膜的抗氧化性能得到改善,对于B1型(Zr,Al)N薄膜,其结构稳定性也得到增强。     

Preparation and characterization of sputtered Cu films containing insoluble Nb

Copper films containing various amounts of insoluble Nb (up to 24.7 at.%) were prepared by r.f. magnetron sputtering. The crystallography and microstructure of the films were investigated for as-deposited and annealed Cu(Nb) thin films. Cu(Nb) thin films are found to consist of non-equilibrium supersaturated solid solution of Nb in Cu with a nanocrystalline microstructure. X-ray diffraction and scanning electron microscope analyses revealed a reduction in the grain sizes of the films with increasing Nb content in the films leading to a grain refinement. The electrical resistivity of as-deposited and annealed Cu(Nb) thin films is found to be low for an Nb content 2.7 at.%. Significant drops in the resistivity were observed for the high Nb contents after annealing at 530 °C which may be due to grain growth and formation of Nb-bearing phase in the film. Microhardness of the films was found to increase with the Nb concentration due to the combined effects of grain refinement and the solute strengthening of Nb.     

Synthesis and characterization of zirconium oxynitride ZrOxNy coatings deposited via unbalanced DC magnetron sputtering

A study of structure, morphology, and corrosion resistance was performed on zirconium oxynitride thin films deposited on 304 and 316 stainless steels by the DC sputtering magnetron unbalance technique. Structural analysis was carried out using X-ray diffraction (XRD), while morphological analysis was performed by scanning electron microscopy (SEM), atomic force microscopy (AFM), and transmission electron microscopy (TEM). These studies were performed as a function of deposition time via DC sputtering at room temperature (287 K) with an Ar/air flow ratio of 3.0 and a total deposition time of 30 min. The oxynitride films were grown with cubic crystalline structures Zr₂ON₂ and preferentially oriented along the (222) plane. Chemical analysis determined that in the last 5.0 nm, the Zr coatings present the following spectral lines: Zr3d_3/2 (184.6 eV) and 3d_5/2 (181.7 eV), O1s (531.3 eV), and N1s (398.5 eV).     

AlN/WAlN/W太阳能选择性吸收多层薄膜研究

采用全封闭磁场的非平衡态磁控溅射系统,以纯金属为靶材,制备了AlN/WAlN(多层)/W薄膜。X射线掠射(GID)、扫描电镜(SEM)以及分光光度计等测试手段分析薄膜的相结构、表面形貌以及吸收光谱等特性。结果表明,薄膜沉积设备性能稳定,W、Al靶材溅射率高。获得AlN/WAlN(多层)/W薄膜中各层薄膜表面质地都较均匀,且为多晶态或纳米晶薄膜。该结构膜系对波长在200～2000nm范围内的光波有较高的吸收效果,平均吸收率可达96%以上,吸收性能优异。     

The effect of deposition parameters on the properties of yttria-stabilized zirconia thin films

Yttria-stabilized zirconia (YSZ) films were deposited by RF magnetron sputtering in order to examine the effects of sputtering conditions on the properties of the resulting thin-films. X-ray diffraction (XRD), Rutherford backscattering spectroscopy (RBS) and scanning electron microscopy (SEM) were used to characterize the films. Additionally, films were deposited on alumina bars to examine the effect of the coatings on the strength of a brittle substrate. RBS analysis indicated that the ratio of oxygen to zirconium in the films varied from 1.84 to 2.10. XRD showed that there was a wide variation in the amount of monoclinic and tetragonal phases that appeared to be related to the O:Zr ratio. Despite these variations, there was no significant difference found in flexural strength found among the groups of alumina bars that were coated with YSZ. The likely cause is the columnar grain morphology of the deposited thin-films, which does not allow strengthening mechanisms to become operative.     

Component redistribution during Nb and In/Nb film growth on single-crystal silicon

The component redistribution during the growth of Nb and In/Nb films on single-crystal silicon has been studied by Rutherford backscattering spectroscopy and X-ray diffraction. The results indicate that magnetron sputtering of indium onto niobium films gives rise to mass transfer across the Nb/Si interface and to niobium and silicon heterodiffusion, accompanied by chemical reactions and the formation of silicides. The likely reason for this is the generation of defects during the magnetron sputtering of indium.