Metallic thin film depth measurements by X-ray microanalysis

In this study, a low-cost technique, energy dispersive spectroscopy (EDS), was used to explore the application of X-ray microanalysis in depth determination of metallic films. Al, Ni and Au films with varied thicknesses from 50 to 400 nm were deposited on silicon (Si) substrates by magnetron sputtering. Electron beam energies ranging from 4 to 30 keV were applied while other parameters were kept constant to determine the electron beam energy required to penetrate the films. The effect of the atomic number of the metallic films on the penetration capability of the electron beam was investigated. Based on the experimental results, mathematical models for Al, Ni and Au films were established and the interaction volume was simulated using a Monte Carlo program. The simulations are in good agreement with the experimental results. Al/Ni/Au multilayers were also studied.     

GaN基紫光LED的高反射率p型欧姆接触

研究用于GaN基大功率倒装焊(Flip-chip)紫光LED(UV-LED)的高反射率p型欧姆接触的电学和光学性能。用磁控溅射的方法在GaN基LED外延片表面沉积了不同厚度Ag,Al,Au和Pd四种金属,测量了样品的反射率和透射率。结合同步辐射高强度X射线衍射和AFM对金属薄膜的晶体结构进行分析,并对表面形貌进行了观测,对由金属薄膜构成的多层膜结构及其对光反射率的作用机理进行了研究。测量结果表明,在入射光波长为400nm时,Ni/Au/Ag和Ni/Au/Al电极的反射率比Ni/Au的反射率提高了三倍。同时与p-GaN有良好的欧姆接触特性。     

热处理对ZnO/Au薄膜结构和压电特性的影响

通过射频磁控溅射在氧化硅片表面沉积ZnO/Au薄膜,并通过不同的热处理方式对薄膜进行退火。为了研究退火对ZnO/Au薄膜结构和压电特性的影响,采用X射线衍射分析（XRD）、光学显微镜、场发射扫面电镜（FESEM）和压电力分析仪对薄膜退火前后的材料特性进行了分析。研究发现,热处理能够改善ZnO/Au薄膜的结晶质量。特别是在氮气保护氛围下慢速退火后,薄膜结晶质量有明显改善。但是,热处理导致了薄膜的压电系数d33和d31降低。分析认为,热处理过程中Au原子在ZnO中的易迁移特性破坏了ZnO/Au薄膜的压电性能。     

高反射率p-GaN欧姆接触电极

根据光学薄膜原理计算了GaN/Ti/Ag、GaN/Al和GaN/Ni/Au/Ti/Ag、GaN/Ni/Au/Al多层电极结构的反射率,得出Ag基和Al基反射电极均能在全角范围内提供较高的反射率。实验测量结果表明,反射率能高于80%的Ag基反射电极,具有低欧姆接触的电学特性。并将GaN/Ni/Au/Ti/Ag多层反射电极应用在上下电极结构的GaN基LED中。实验上采用两步合金法获得了低接触电阻、高反射率的电极结构,并引入Ni/Au覆盖层克服了Ag高温时的团聚和氧化现象。解决了Ag电极的稳定性问题,显著地提高了LED的出光效率,成功制备了具有上下电极结构的GaN基LED管芯。     

High quality ZnS/Au/ZnS transparent conductive tri-layer films deposited by pulsed laser deposition

ZnS/Au/ZnS tri-layer films were deposited on quartz glass substrates by pulsed laser deposition. The influence of Au layer thickness on optical and electrical properties of the tri-layer ZnS/Au/ZnS was studied. X-ray diffractometer (XRD) and scanning electron microscope were employed to characterize the crystalline structure and surface morphology of the tri-layer films. Hall measurements, ultraviolet and visible spectrophotometer, four-point probe were used to explore the optoelectronic properties of the ZnS/Au/ZnS. The increase of Au layer thickness resulted in the decreased resistivity, the increased carrier concentration, and the declined transmittance in the visible light region.     

Use of TiB2 diffusion barriers for Ni/Au ohmic contacts on p-GaN

The use of a TiB₂ diffusion barrier for Ni/Au contacts on p-GaN is reported. The annealing temperature (25-950 °C) dependence of ohmic contact characteristics using a Ni/Au/TiB₂/Ti/Au metallization scheme deposited by sputtering were investigated by contact resistance measurements and auger electron spectroscopy (AES). The as-deposited contacts are rectifying and transition to ohmic behavior for annealing at ≥500 °C . A minimum specific contact resistivity of ∼3 × 10⁻⁴ Ω cm⁻² was obtained after annealing over a broad range of temperatures (800-950 °C for 60 s). The contact morphology became considerably rougher at the higher end of this temperature range. AES profiling showed significant Ti and Ni outdiffusion through the TiB₂ at 800 °C. By 900 °C the Ti was almost completely removed to the surface, where it became oxidized. Use of the TiB₂ diffusion barrier produces superior thermal stability compared to the more common Ni/Au, whose morphology degrades significantly above 500 °C.     

金镍复合膜上碳纳米管的定向生长及生长过程中金的作用

以金镍复合膜作催化剂，在96%的高氢气浓度下实现了碳纳米管的定向生长，并对其生长过 程进行了深入探讨.结果表明，高氢气浓度下碳纳米管生长的实现与本实验所选用的催化剂 ——金镍复合膜有密切关系.催化剂中金的参与，促进了碳在催化剂中的扩散，提高了碳在 催化剂中的活度.与催化剂中没有金的情况相比较，金的参与有利于镍吸收气氛中的碳，从 而使镍更容易达到碳饱和，有利于在高的氢气浓度下实现碳纳米管的定向生长. 关键词： 金镍复合膜 高氢气浓度 原子氢 碳活度     

磁控溅射沉积铝/贫铀与金/贫铀镀层的界面研究

采用磁控溅射技术沉积制铝/贫铀/铝(Al/DU/Al)、金/贫铀/金(Au/DU/Au) "三明治" 薄膜样品. 利用高分辨扫描电镜、 X射线衍射仪、X射线光电子能谱仪、 扫描俄歇微探针对Al/DU/Al, Au/DU/Au样品的Al/DU, Au/DU界面行为进行表征与研究. 结果表明: 沉积态DU层以柱状晶生长; Al/DU界面扩散明显, 物理扩散过程中伴随着Al, DU化学反应形成Al₂U, Al₃U金属化合物; 金属化合物的形成导致界面处Al 2p电子结合能向高能端移动, U 4f电子向低能端移动; 微量O在Al/DU界面处以Al₂O₃及铀氧化物形式存在; DU镀层中以铀氧化形式存在; 沉积态的Au/DU界面扩散为简单的物理扩散, 团簇效应导致Au/DU界面处Al 2p, U 4f电子结合能均向高能端移动; 在Au/DU界面及DU镀层中, 微量O以铀氧化物形式存在; Al/DU界面扩散强于Au/DU; 相同厚度的Al, Au保护镀层, Al镀层保护效果优于Au镀层. 关键词： Al/DU界面 Au/DU界面 磁控溅射 界面扩散     

Dumbbell to Core–Shell Structure Transformation of Ni–Au Nanoparticle Driven by External Stimuli

Conversion of CO₂ gas to CO fuels is one of the most promising solutions for the increasing threat of global warming and energy crisis. The efficient catalyst Ni–Au dumbbell converting CO₂ into CO at elevated temperatures has high CO product selectivity; however, the accompanied atomic diffusion and subsequent surface reconstruction affect the catalytic efficiency of chemical reaction. Atomic scale characterization of structural evolution of the catalyst, which is essential to correlate the functional mechanism to active catalyst surfaces, is yet to be studied. Here, in situ transmission electron microscopy experiments and atomistic simulations are performed to characterize the structural evolution of Ni–Au dumbbell nanoparticles under two different external stimuli. In the condition of high temperature and vacuum, the Ni–Au nanostructure reveals a clear shape reconstruction from the initial dumbbell to core–shell‐like, which is induced by capillary force to minimize free surface energy of the system. The shape transformation involves two stages of processes, initial fast Au diffusion followed by slow source‐controlled diffusion. At ambient temperature, the combination of CO₂ and electron flux surprisingly induces analogous structural transformation of Ni–Au nanostructure, where the associated chemical reaction and CO absorption stimulate the Au migration on Ni surface. Such surface reconstruction can be widely present in catalytic reactions in different environmental conditions, and the results herein demonstrate the detailed processes of Ni–Au structure evolution, which provide important insights for understanding the catalyst performance.     

Thermal stability and electrical characteristics of NiSi films with electroplated Ni(W) alloy

In this study, an electroplating method to deposited Ni, crystalline NiW(c-NiW), amorphous NiW (a-NiW) films on P-type Si(1 0 0) were used to form Ni-silicide (NiSi) films. After annealed at various temperatures, sheet resistance of Ni/Cu, c-NiW/Cu and a-NiW/Cu was measured to observe the performance of those diffusion barrier layers. With W added in the barrier layer, the barrier performance was improved. The results of XRD and resistance measurement of the stacked Si/Ni(W)/Cu films reveal that Cu atom could diffuse through Ni barrier layer at 450 °C, could diffuse through c-NiW at 550 °C, but could hardly diffuse through a-NiW barrier layer. c-NiW layer has a better barrier performance than Ni layer, meanwhile the resistance is lower than a-NiW layer.     

High-temperature application of the low-emissivity Au/Ni films on alloys

The 200 nm-thickness Ni film was imposed as the diffusion barrier layer between the Au film and the alloy substrate to improve the low-emissivity durability of the Au film at high temperature. The results show that the Au/Ni multilayer films still kept low emissivity after working at 600 °C for 200 h. It was concluded that the Ni interlayer effectively retarded the diffusion between gold film and the metal alloy below 600 °C.     

CdTe太阳电池的不同背电极和背接触层的特性研究

用Ni替代Au来作为CdTe太阳电池的背电极，比较了Ni,Ni/Au,Au/Ni及Au背电极对电池性能的影响.发现Ni作为背电极和ZnTe/ZnTe:Cu复合层接触，电池的开路电压V_oc略有降低，填充因子FF有增有减，变化幅度不大，但因短路电流I_sc有较大的提高，转换效率η平均增长4％.测试了不同背电极的CdTe太阳电池的暗I-V和C-V特性，对背电极剥离后的样品进行了XPS测试分析.结果表明，Ni扩散到ZnTe/ZnTe:Cu复合层的深度比Au多，且大多呈离子态，与ZnTe/ZnTe:Cu复合层中的富Te离子形成Ni_xTe，提高了掺杂浓度，使电池性能获得改善. 关键词： 金属背电极 复合背接触层 转换效率 CdTe太阳电池     

Study of Ti/Au,Ti/Al/Au,and Ti/Al/Ni/Au ohmic contacts to <Emphasis Type="Italic">n</Emphasis>-GaN

The contacts of Ti/Au, Ti/Al/Au, and Ti/Al/Ni/Au films deposited on n-GaN were studied by current–voltage (I–V) and transmission-line-method measurements. The effect of annealing temperature on specific contact resistivity has been investigated by changing the annealing temperature from 400 to 900 °C. Ti/Al/Au and Ti/Al/Ni/Au films were superior to the bilayer (Ti/Au) in ohmic contact characteristics and thermal stability. The Ti/Al/Ni/Au composite showed the best thermal stability due to the fact that Ni plays a more important role than the alloy of Ti/Al in preventing the interdiffusion of Ti, Al, and Au. The lowest contact resistivity (10^-7cm²) to n-GaN was obtained for the Ti/Al/Ni/Au sample by short-time/high-temperature annealing. The formation mechanism of ohmic contacts to n-GaN is also discussed. PACS 73.40.Cg; 73.61.Ey     

Study of Ni/Si(1 0 0) solid-state reaction with Al addition

The characteristics of Ni/Si(1 0 0) solid-state reaction with Al addition (Ni/Al/Si(1 0 0), Ni/Al/Ni/Si(1 0 0) and Al/Ni/Si(1 0 0)) is studied. Ni and Al films were deposited on Si(1 0 0) substrate by ion beam sputtering. The solid-state reaction between metal films and Si was performed by rapid thermal annealing. The sheet resistance of the formed silicide film was measured by four-point probe method. The X-ray diffraction (XRD) was employed to detect the phases in the silicide film. The Auger electron spectroscopy was applied to reveal the element profiles in depth. The influence of Al addition on the Schottky barrier heights of the formed silicide/Si diodes was investigated by current-voltage measurements. The experimental results show that NiSi forms even with the addition of Al, although the formation temperature correspondingly changes. It is revealed that Ni silicidation is accompanied with Al diffusion in Ni film toward the film top surface and Al is the dominant diffusion species in Ni/Al system. However, no Ni_xAl_y phase is detected in the films and no significant Schottky barrier height modulation by the addition of Al is observed.     

Growth behavior and magnetic property of electroless NiCoFeP films

The electroless NiCoFeP films were deposited on a silicon substrate in a bath containing Ni²⁺, Co²⁺, and Fe²⁺ ions with a concentration ratio of 1:1.9:1.2. These films were characterized by using transmission electron microscope, energy dispersive X-ray spectrometer, and alternating gradient magnetometer for their microstructure, crystal structure, and magnetic properties. The result showed that the film deposited at the initial stage (about 10 s) consists of only one phase with a crystal structure of FCC Ni and a composition about Ni (69 at%), Co (19 at%), Fe (4 at%), and P (7 at%); The film deposited at the latter stage (about 30 s) consists of two phase, one is similar to that of initial stage and the other has crystal structure of HCP Co with a composition about Ni (35 at%), Co (44 at%), Fe (19 at%), and P (2 at%). The saturation magnetization and coercivity of electroless NiCoFeP films vary from 525 to 1546 emu/cm³ [0.68–2.01 T] and from 51.44 to 88.5 Oe [4.09–7.04 kA/m], respectively.     

High reflective p-GaN/Ni/Ag/Ti/Au Ohmic contacts for flip-chip light-emitting diode (FCLED) applications

The fabrication of high reflective Ni/Ag/(Ti, Mo)/Au Ohmic contacts for flip-chip light-emitting diode (FCLED) are proposed and considered, Ni/Ag/Au Ohmic contacts are also fabricated to compare their resulting reflectivities. From secondary ion mass spectrometry (SIMS) depth profiles, it indicates that the Au in-diffusion occurs in Ni/Ag/Au contacts after annealing. It is considered that Au in-diffusion, which is intermixed with Ag, Ni and GaN in Ni/Ag/Au contacts after annealing, is responsible for the resulting low reflectance (63% at the wavelength of 465 nm). To avoid Au in-diffusion and enhance the reflectivity, a diffusion barrier metal (Ti or Mo) between Ni/Ag and Au is fabricated and examined. It is demonstrated and found that an insertion of diffusion barrier metal of Ti enables to block Au diffusion effectively and also improve the reflectivity significantly, up to 93%.     

Electron transmission measurements of electron mean free path in supported thin films from 1–5 keV

Measurements are made of the transmission of medium energy electrons through in vacuo deposited films in order to determine the inelastic electron mean free path as a function of energy. Films of Al, Ge and Au are deposited in small increments on 20–30 Å carbon substrates supported by “holey” carbon films. The no-loss electron current is measured for each thickness as a continuous function of incident energy in the range of 1–5 keV. Although this preliminary experiment does not result in a precise separation of elastic and inelastic scattering effects, the attenuation lengths estimated are in reasonable agreement with measured and calculated in-elastic mean free paths. Elastic scattering cross sections appear to be smaller than estimated by simple theory.     

XPS study of low temperature diffusion in Au/Ni couples in the presence of arsenic

X-ray photoelectron spectroscopy, XPS, has been utilized to determine the low temperature grain boundary diffusion of nickel through gold thin films by means of surface accumulation. Surface accumulation is aided by a rapid oxidation of the nickel diffusant at the surface by arsenic vapor at very low (<10^-8 Torr) pressure causing a rapid accumulation of nickel arsenide product. The initial low temperature diffusion parameters of Au/Ni couples were measured in situ without interrupting the reaction-accumulation process. Accumulation and diffusion rates were obtained for temperatures ranging from 110 to 147° C. A discontinuity in an otherwise linear accumulation was observed after approximately 150 min. Evidence suggests that surface effects become rate limiting at this point.     

Effect of gas pressure on the growth of selenium thin films by pulsed laser deposition

The effect of an inert gas pressure on the structure of selenium thin films has been systematically investigated in the pulsed laser deposition process. The ablated material is deposited on Au (111) gold thin films for its characterization by atomic force microscopy (AFM). Analysis of the surface morphology shows that instead of the formation of a uniform Se thin film on top of Au (111) terraces, as it occurs in high vacuum, the film grows as two dimensional ellipsoid shaped aggregates. The size of these Se aggregates increases significantly with the gas pressure and reaches a maximum at pressures of 1.5 Torr, and subsequently decreases with further increase of the gas pressure. This effect is probably due to the fact that the kinetic energy of the impinging species decreases as pressure increases, thus impeding diffusion on the substrate surface. However, further increase in the pressure prevents the Se species from being deposited on the substrate resulting in a decrease in size of the aggregates. PACS 81.07; 68.37.P; 81.16.M     

Implications in the use of sputtering for layer removal: the system Au on Si

Au films deposited on Si substrates have been sputtered by 20 and 100 keV Ar bombardment, respectively. Bombardment-induced intermixing of Au and Si was observed at film thicknesses considerably larger than the projectile range. Due to radiation-enhanced diffusion, the partial sputtering yield of Au from Si-Au alloys decreases with increasing fluence. Complete removal of Au from Si is impossible if Ar ions are used for sputtering.