水对纳米掺钯WO3薄膜气致变色性能的影响

以W粉为原材料,通过溶胶凝胶法结合提拉镀膜法制备了掺钯的气致变色WO3纳米多孔薄膜,并采用不同温度对该薄膜进行了热处理;最后制作成简易的气致变色窗。分别采用傅立叶红外光谱仪(FT-IR)、原子力显微镜(AFM)表征了薄膜中水的存在和薄膜的表面形貌,采用紫外/可见/近红外分光光度计对薄膜致褪色过程的透射率随时间的变化进行原位动态的测试,分析了不同阶段的水的存在对薄膜气致变色性能的影响。研究结果表明:随着气致变色循环次数的增加,薄膜生成水逐渐增加,破坏了薄膜的表面结构,堵塞了薄膜的孔洞,使薄膜气致变色时间延长,但不影响薄膜的致色深度;环境吸附水对薄膜有毒化作用,既延长了薄膜的气致变色的时间也使气致变色深度降低;而适量的薄膜结构水的存在有利于提高薄膜的气致变色速率。     

Material and sensing properties of Pd-deposited WO3 thin films

The physicochemical and electrical properties of Pd-deposited WO3 thin films were investigated as a function of Pd thickness, annealing temperature, and operating temperature for application as a hydrogen gas sensor. WO3 thin films were deposited on an insulating material using a thermal evaporator. X-ray diffractometry (XRD), field emission scanning electron microscopy (FE-SEM), atomic force microscopy (AFM), and X-ray photoelectron spectroscopy (XPS) were used to evaluate the crystal structure, microstructure, surface roughness, and chemical property of the films, respectively. The deposited films grew into polycrystalline WO3 with a rhombohedral structure after annealing at 500 degrees C. Adding Pd had no effect on the crystallinity, but suppressed the growth of WO3 grains. The Pd was scattered as isolated small spherical particles of PdO2 on the WO3 thin film after annealing at 500 degrees C, while it agglomerated as irregular large particles or diffused into the WO3 after annealing at 600 degrees C. PdO2 reduction under H2 and reoxidation under air were dependent on both the Pd deposition thickness and annealing conditions. The WO3 thin film with a 2-nm-thick Pd deposit showed a good response and recovery to H2 gas at a 250 degrees C operating temperature.     

Ultrafast coloring-bleaching performance of nanoporous WO3-SiO2 gasochromic films doped with Pd catalyst

The gasochromic performance and durability of WO(3)-based films can be improved by doping SiO(2) particles within WO(3) matrix forming nanoporous supporting network and dispersing Pd catalyst inside films with enhanced catalytic activity. Nanoporous WO(3)-SiO(2) composite films loaded with Pd catalyst were prepared by sol-gel dip-coating process and served as an active chromogenic layer to fabricate a double-glazed gasochromic device. The structure, morphology, optical properties and gasochromic performance of WO(3)-SiO(2) films were fully investigated. The WO(3)-SiO(2) films exhibit excellent gasochromic performance with ultrafast coloring rate of 14.8% per second (%/s) (WO(3): 2.84%/s) and bleaching rate of 44.1%/s (WO(3): 7.18%/s). The transmittance changed between 17.8 and 74.6% during coloring-bleaching cycles, and totally reversibility and stability were achieved.     

纳米掺钯WO3薄膜及气致变色性能研究

以钨粉和双氧水为原料,采用溶胶-凝胶技术结合提拉镀膜法,制备了纳米结构掺钯气致变色WO3薄膜;分析了薄膜的折射率、厚度、结晶度、红外特性和表面形貌随温度变化特性;研究了薄膜的气致变色性能。研究结果表明,纳米掺钯气致变色WO3薄膜有着良好的气致变色特性。重点讨论了薄膜结构、薄膜水含量以及薄膜钯含量对薄膜变色效率的影响。     

Platinum and palladium high-temperature transducers on langasite

There is a pressing need for the fabrication of surface acoustic wave (SAW) devices capable of operating in harsh environments, at elevated temperature and pressure, or under high-power conditions. These SAW devices operate as frequency-control elements, signal-processing filters, and pressure, temperature, and gas sensors. Applications include gas and oil wells, high-power duplexers in communication systems, and automobile and aerospace combustion engines. Under these high-temperature and power-operating conditions, which can reach several hundred degrees Centigrade, the typically fabricated aluminum (A1) thin film interdigital transducer (IDT) fails due to electro and stress migration. This work reports on high temperature SAW transducers that have been designed, fabricated, and tested on langasite (LGS) piezoelectric substrates. Platinum (Pt) and palladium (Pd) (melting points at 1769 degrees C and 1554.9 degrees C, respectively) have been used as thin metallic films for the SAW IDTs fabricated. Zirconium (Zr) was originally used as an adhesion layer on the fabricated SAW transducers to avoid migration into the Pt or Pd metallic films. The piezoelectric LGS crystal, used as the substrate upon which the SAW devices were fabricated, does not exhibit any phase transition up to its melting point at 1470 degrees C. A radio frequency (RF) test and characterization system capable of withstanding 1000 degrees C has been designed and constructed. The LGS SAW devices with Pt and Pd electrodes and the test system have been exposed to temperatures in the range of 250 degrees C to 750 degrees C over periods up to 6 weeks, with the SAW devices showing a reduced degradation better than 7 dB in the magnitude of transmission coefficient, /S21/, with respect to room temperature. These results qualify the Pt and Pd LGS SAW IDTs fabricated for the above listed modern applications in harsh environments.     

Tin oxide nanocluster hydrogen and ammonia sensors

We have prepared sensitive hydrogen and ammonia sensors from thin films of tin nanoclusters with diameters between 3 and 10?nm. By baking the samples at 200?°C in ambient air the clusters were oxidized, resulting in very stable films of tin oxide clusters with similar diameters to the original Sn clusters. By monitoring the electrical resistance, it is shown that the cluster films are highly responsive to hydrogen and ammonia at relatively low temperatures, thereby making them attractive for commercial applications in which low power consumption is required. Doping of the films by depositing Pd on top of the clusters resulted in much improved sensor response and response times. It is shown that optimal sensor properties are achieved for very thin cluster films (a few monolayers of clusters).     

TaSi2 nanowires: A potential field emitter and interconnect

TaSi2 nanowires have been synthesized on a Si substrate by annealing NiSi2 films at 950 degrees C in an ambient containing Ta vapor. The nanowires could be grown up to 13 microm in length. Field-emission measurements show that the turn-on field is low at 4-4.5 V/microm and the threshold field is down to 6 V/microm with the field enhancement factor as high as 1800. The metallic TaSi2 nanowires exhibit excellent electrical properties with a remarkable high failure current density of 3 x 10(8) A cm(-2). In addition, effects of annealing temperatures and capability of metal silicide mediation layer on the growth of nanowires are addressed. This simple approach promises future applications in nanoelectronics and nano-optoelectronics.     

Structural and chemical stability of Ta–Si–N thin film between Si and Cu

Thermal stability and barrier performance of reactively sputter deposited Ta–Si–N thin films between Si and Cu were investigated. RF powers of Ta and Si targets were fixed and various N₂/Ar flow ratios were adopted to change the amount of nitrogen in Ta–Si–N thin films. The structure of the films are amorphous and the resistivity increases with nitrogen content. After annealing of Si/Ta–Si–N(300 Å)/Cu(1000 Å) structures in Ar–H₂ (10%) ambient, sheet resistance measurement, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and Auger electron spectroscopy (AES) were employed to characterize barrier performance. Cu₃Si and tantalum silicide phase are formed at the same temperature, and the interdiffusion of Si and Cu occurs through the local defect sites. In all characterization techniques, nitrogen in the film appears to play an important role in thermal stability and resistance against Cu diffusion. A 300 Å thick Ta₄₃Si₄N₅₃ barrier shows the excellent barrier property to suppress the formation of Cu₃Si phase up to 800°C.     

Piezoelectric tantalum pentoxide studied for optical tunable applications

Piezoelectric transparent thin films are of great interest for use in tunable filters. We present experimental results on Ta2O5 single layers coated on fused-silica substrates with an electron-beam deposition process. Above 450 degrees C, coatings change from an amorphous to a polycrystallized structure. When this structure shows a preferred orientation matching the piezoelectric tensor of the Ta2O5 crystal and the external electric field, variation in the piezoelectric layer thickness is expected. We detail experimental results in terms of optical (spectrophotometric and scattering measurements) and nonoptical characterizations (x-ray diffraction and scanning electron microscopy). Then the resultant thickness variation under oscillating applied voltage is measured with an extrinsic Fabry-Perot interferometer setup.     

High Coercive NdFeB Thin Film Obtained by Diffusion Annealing

1. IntroductionSince the discovery of the high performance NdFeB permanent magnetll'2] ) there has been much interest in the magnetic properties and its applications.In most of the applications, bulk NdFeB magnetsare used. Due to the dependence of magnetic properties on ndcrostructure, the systematical change ofthe length scales and illtergranular phase, such asin thin films, have been illterested to optimize theirmagnetic properties. The film magnets are made bysputteringl3], MBEI4] and l…     

Effect of under-layer treatment of Ta/TaN barrier film on corrosion between Cu seed and Ta in chemical-mechanical-polishing slurry

Tantalum/tantalum nitride (Ta/TaNx) composite film is widely used as a copper (Cu) diffusion barrier layer. In order to reduce via-resistance, an additional argon (Ar) re-sputtering process is used to thin the barrier thickness at the feature bottom. In this study, the effect of Ar re-sputtering of the under-layer of TaNx barrier films on the corrosion between Cu seeds and upper Ta films in chemical-mechanical-polishing (CMP) slurries was investigated. The results show that Ar re-sputtering of the under-layer of the TaNx barrier has a strong influence on the corrosion of Cu seeds and Ta films. The equivalent circuit, simulated using data from electrochemical analysis, reveals changes in resistance and capacitance elements of the Cu-Ta electrochemical system, proving that the phase transformation of upper Ta films under different TaNx conditions leads to different degrees corrosion of Cu seeds and the Ta films.     

Red shift for CdTe nanoparticle thin films and suspensions during heating

The work that we have conducted shows that temperature affects the wavelength of light emitted from CdTe nanoparticle clusters that are in a suspension or deposited into thin films via a layer-by-layer process. Compared with the stock suspension, the films show an initial photoluminescent shift, of circa 6-8 nm to the red, when the particles are deposited. A shift of circa 6-8 nm is also seen when the suspensions are first heated to 85 degrees C from room temperature (20 degrees C) having been stored in a fridge at 5 degrees C. This shift is non-recoverable. With continual cycling from room temperature to 85 degrees C the suspensions show a slight tendency for the emission to move increasingly to the red; whereas the films show no such tendency. In both cases, the range in emission is ca 10 nm from the room temperature state to 80 degrees C. The intensity of the emission from the film drops abruptly (ca 50% reduction) after one cycle of heating; in the suspension there is an initial increase (ca 3-5% increase) in intensity before it decays. We see that the shift towards the red has been attributed to energy transfer or a rearrangement of the packing of the particles in the thin films. After conducting analysis of the films using scanning probe microscopy we have determined that a change in the morphology is responsible for the permanent shift in emission wavelength associated with prolonged heating. The influence of traps has not been ruled out, but the morphological change in the samples is very large and is likely to be the dominating mechanism affecting change for the red shift at room temperature.     

Growth of highly c-axis oriented aluminum nitride thin films on β-tantalum bottom electrodes

We have investigated the influence of tantalum (Ta) bottom electrodes on the crystallinity and crystal orientation of aluminum nitride (AlN) thin films. AlN thin films and Ta electrodes were prepared by using rf magnetron sputtering method. The crystal structure of the Ta electrodes was tetragonal (β-Ta, a metastable phase) at room temperature. The crystallinity and orientation of the AlN thin films and Ta electrodes strongly depended on sputtering conditions. Especially, the crystallinity and crystal orientation of the Ta electrodes were influenced by their film thickness and the substrate temperature. When the thickness of the Ta bottom electrodes was 200 nm and the substrate temperature was 100 °C, the AlN thin films indicated high c-axis orientation (the full width at half maximum of rocking curve of 3.9°). The crystal orientation of the AlN film was comparable to that of AlN thin films deposited on face centered cubic (fcc) lattice structure metal, such as Au, Pt and Al, bottom electrodes.     

A micromachined calorimetric gas sensor: an application of electrodeposited nanostructured palladium for the detection of combustible gases

Palladium films with regular nanoarchitectures were electrochemically deposited from the hexagonal (H1) lyotropic liquid crystalline phase of the nonionic surfactant octaethyleneglycol monohexadecyl ether (C16EO8) onto micromachined silicon hotplate structures. The H1-e Pd films were shown to have high surface areas (approximately 28 m2 g(-1)) and to act as effective and stable catalysts for the detection of methane in air on heating to 500 degrees C. The response of the H1-e Pd-coated planar pellistors was found to be linearly proportional to the concentration of methane between 0 and 2.5% in air with a detection limit below 0.125%. Our results show that the electrochemical deposition of nanostructured metal films offers a promising approach to the fabrication of micromachined calorimetric gas sensors for combustible gases.     

Temperature-compensated RC networks developed using TaAlN thin films

Temperature compensation is of primary concern in the development of precision thin film hybrid circuits. Circuits developed with matching temperature coefficients between resistor and capacitor elements exhibit stability against variations in the ambient temperature. In this paper the performance of temperature-compensated RC networks developed using TaAlN thin films is described. These films are obtained by co-sputtering a Ta/Al bimetallic target in an N₂Ar reactive atmosphere. The results of tests conducted on circuits made with these new films are also reported.     

反应射频磁控溅射法制备HfTaO薄膜的热稳定性和光学性能

采用反应射频磁控溅射技术制备HfTaO薄膜,利用X射线衍射(XRD)分析了薄膜的微结构,通过紫外-可见光分光光度计测量了薄膜的透过谱,计算了薄膜的折射率和禁带宽度,利用原子力显微镜观察了薄膜的表面形貌。结果表明,随着Ta掺入量(10%,26%,50%)的增加,HfTaO薄膜的结晶化温度分别为800、900、950℃,Ta掺入量继续增加到72%,经过950℃退火处理的HfTaO薄膜仍然保持非晶态,具有优良的热稳定性。AFM形貌分析显示非晶HfTaO薄膜表面非常平整。在550nm处薄膜折射率n随着Ta掺入量的增大而增大,n的变化区间为1.90～2.15。同时HfTaO薄膜的光学带隙Eg随着Ta掺入量的增大而逐渐减小,Eg的变化区间为4.15～5.29eV。     

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.     

Effect of Si target sputtering power on diffusion barrier properties of Ta–Si–N thin films

Abstract

Ta–Si–N thin films and Cu/Ta–Si–N thin films were deposited on p type Si(111) substrates by magnetron reactive sputtering. Then the films were characterised by four point probe sheet resistance measurement, AFM, SEM and XRD respectively. According to the XRD results, the authors found that the crystallisation of Ta nitrides in Ta–Si–N/Si thin films is suppressed effectively when fabricated by a high Si target sputtering power. As the Si target power varies, the failure temperature of Cu/Ta–Si–N/Si is changed. The sample fabricated by the Si target power of 200 W fails after 800°C rapid thermal annealing and it has the highest failure temperature. The investigation of failure mechanism shows that Cu atoms diffuse through grain boundaries or amorphous structure of the Ta–Si–N barrier, and react with Si to form Cu–Si phase. And it causes the failure of the barrier.     

In-situ observations of stress-induced thin film failures

In this work, the failure modes of thin films under thermo-mechanical treatments were observed via in-situ white beam X-ray topography. The in-situ experiments were carried out using an experimental setup on Beamline 2-2 at the Stanford Synchrotron Radiation Laboratory. Magnetron sputtered polycrystalline thin films of Ta and CrN on Si substrates were selected for the present study due to their disparate states of intrinsic residual stresses: the Ta film was anisotropically compressive and the CrN film was isotropically tensile. Under a similar heating-cooling cycle in air, the two types of films exhibited distinct failure modes, which were observed in-situ and in a quasi-real-time fashion. The failures of the samples have been interpreted based on their distinctive growth stress states, superimposed on the additional stress development associated with different forms of thermal instabilities upon heating. These included the formation of oxide for the Ta/Si sample, which led to an increase in compressive stress, and a phase change for the CrN/Si sample, which caused the isotropic stress in the film to become increasingly tensile.     

The influences of rapid-thermal annealing on the characteristics of Sr0.6Ba0.4Nb2O6 thin film

The Sr0.6Ba0.4Nb2O6 (SBN) thin films were successfully prepared on Pt/Ti/Si and SiO2/Si/Al substrates and crystallized subsequently using rapid thermal annealing (RTA) process in ambient atmosphere for 1 min. The surface morphologies and thicknesses of as-deposited and annealed SBN thin films were characterized by field emission scanning electron microscopy, and the thickness was about 246 nm. As compared with the as-deposited SBN thin films, the RTA-treated process had improved the crystalline structures and also had large influence on the crystalline orientation. When the annealing temperatures increased from 700 degrees C to 900 degrees C, the diffraction intensities of (410) and (001) peaks apparently increased. Annealed at 900 degrees C, the (001) peak had the maximum texture coefficient and SBN thin films showed a highly c-axis (001) orientation. The influences of different RTA-treated temperatures on the polarization-applied electric field (P-E) curves and the capacitance-voltage (C-V) curves were also investigated.