基于飞秒激光加工的马赫-曾德尔干涉氢气传感器

介绍了一种基于光纤微加工的氢气传感技术方案。利用波长为800nm的飞秒激光脉冲在普通单模光纤上加工马赫-曾德尔(M-Z)干涉腔,并采用磁控溅射方法在加工后的M-Z干涉微腔上溅射钯(Pd)膜,制备了一种新型的光纤氢气传感器。分析了加工工艺对微腔干涉效果的影响,选择合适的加工参数以及加工后对微腔进行后续处理,可使微腔的透射光谱的分辨率得到提高。实验研究了腔长为40μm的M-Z干涉传感器分别镀36nm、110nmPd膜后,对氢气的响应。结果表明,在不同的氢气浓度下,镀Pd膜的M-Z干涉传感器都表现出对氢气的敏感特性,随着氢气浓度的增大,透射光谱会向长波长方向偏移,其中Pd膜厚度为110nm比厚度为36nm的传感器对氢气有更好的灵敏度。     

基于WO3- Pd复合膜的D型光纤光栅氢气传感器

采用磁控溅射方法在侧边抛磨的光纤光栅（D型光纤光栅）上溅射40 nm WO3-Pd复合薄膜,制作了D型光纤光栅氢气传感器.40 nm WO3-Pd复合薄膜是由5 nm的WO3、5 nm的WO3/Pd混合膜和30 nm的Pd 薄膜组成.实验中,首先采用射频溅射技术向D型光纤光栅溅射5 nm WO3薄膜,再利用共溅射技术溅射5 nm WO3/Pd混合膜,最后用直流溅射技术溅射30 nm的Pd薄膜.SEM结果显示在多次通氢气后WO3-Pd薄膜仍然具有较好的表面形貌,这说明WO3-Pd复合薄膜具有较好的机械性能.实验结果表明:该氢气传感器具有较好的重复性,同镀有同样氢气敏感膜的普通FBG相比,D型光纤光栅的灵敏度提高了200%|在氢气体积浓度为6%时,D型光纤光栅传感器的波长变化为15pm.     

基于光纤微结构加工和敏感材料物理融合的光纤传感技术

将功能敏感材料与光纤在物理层面进行有机融合,充分发挥光纤传感器在结构集成、材料集成等方面的优势,将有望发展新型的光纤传感器件和系统.本文综述了飞秒激光光纤微加工技术分别在标准的单模光纤和光纤光栅上制备微结构,再结合敏感材料制备技术,实现在物理层面上光纤传感器材料和结构的集成和融合,探索实现新型高性能的光纤传感新技术.     

Hydrogen Permeability of a Foil of Pd–Ag Alloy Modified with a Nanoporous Palladium Coating

Thin films with the composition Pd–23% Ag are obtained via magnetron sputtering. The magnetron sputtering of Pd–50% Zn films with subsequent diffusion annealing and etching of the active component is used to modify the surfaces of palladium–silver films to improve their hydrogen permeability. Modifying the surfaces of the resulting Pd–Ag films using a nanoporous palladium coating with a predominant distribution of particles ranging from 0 to 50 nm allows a hydrogen flux density of up to 0.4 mmol s^?1 m^?2 to be achieved for sufficiently thin palladium membranes (<10 μm) under conditions of low temperature (<90°C) and pressure (<0.6 MPa). Experimental evidence is gathered that under these conditions, the velocity of hydrogen transport is limited by dissociative–associative processes at membrane boundaries and can be greatly (by an order of magnitude) increased, due to acceleration of the limiting stage of the process via the formation of a palladium nanoporous coating on the film’s surface.     

Electrodeposition and magnetic properties of Ni nanowire arrays on anodic aluminum oxide/Ti/Si substrate

Ni nanowire arrays with different diameters have now been extended to directly fabricate in porous anodic alumina oxide (AAO) templates on Ti/Si substrate by direct current (DC) electrodeposition. An aluminum film is firstly sputter-deposited on a silicon substrate coated with a 300 nm Ti film. AAO/Ti/Si substrate is synthesized by a two-step electrochemical anodization of the aluminum film on the Ti/Si substrate and then used as template to grow Ni nanowire arrays with different diameters. The coercivity and the squareness in parallel direction of Ni nanowires with about 10 nm diameters are 664 Oe and 0.90, respectively. The Ni nanowire arrays fabricated on AAO/Ti/Si substrates should lead to practical applications in ultrahigh-density magnetic storage devices because of the excellent properties.     

Study on the thermoelectric properties of porous Bi-Te films deposited using thermal evaporation on AAO template

The application of thermoelectric films is limited to retain the temperature gradient. In this study, the Bi-Te films are deposited on the AAO template with a pore size of 100 nm using thermal evaporation. The results show that the conductive types of the Bi-Te film are tuned by source temperature. The power factor of the p-type porous film decreases 36% by comparing to that of the p-type nonporous film (1020 μW/mK² at 250 °C). Meanwhile, the temperature difference in the porous device is maintained and is approximately 5.0 °C. Thus, the maximum output power is achieved in the porous device (about 25 pW), which is 5 times higher than that of the nonporous device. This provides a method to improve the conversion efficiency of thermoelectric film device by maintaining the temperature difference by using porous structure.     

Synthesis of epitaxial Si(100) nanowires on Si(100) substrate using vapor–liquid–solid growth in anodic aluminum oxide nanopore arrays

The synthesis of epitaxial Si nanowires with growth direction parallel to Si [100] on Si(100) substrate was demonstrated using a combination of anodic aluminum oxide (AAO) template, catalytic gold film sandwiched between the template and the Si(100) substrate and vapor-liquid-solid growth using SiH₄ as the Si source. After growing out from the AAO nanopores, most Si nanowires changed their diameter and growth direction into larger diameter and 〈111〉 direction. PACS 81.07.-b; 82.45.Cc     

A highly sensitive and selective hydrogen gas sensor from thick oriented films of MoS2

A new process is developed to fabricate a highly sensitive and selective hydrogen sensor by depositing a partially crystalline and highly oriented film of MoS₂ from its single layer suspension on an alumina substrate. When these films are promoted with some catalysts selected from Pt-group metals (Pt, Pd, Ru or any combination of these metals) they exhibit a high sensitivity and selectivity to hydrogen gas. Unlike other metal oxide sensors which are sensitive to many reducing and oxidizing gases and operate at a temperature of 350 °C or higher; this sensor is highly selective to hydrogen gas and its operating temperature is from 25 to 150°C. The lower operating temperature enhances safety when dealing with hydrogen gas. The sensor response to hydrogen at 120 °C is linear in concentration from 30 to 10⁴ ppm with a 10 to 30 second response time and a 45 to 90 second recovery time. Above 10⁴ ppm the sensor is still linear but the slope of conductance versus hydrogen concentration changes.     

纳米压印多孔硅模板的研究

纳米压印模板通常采用极紫外光刻、聚焦离子束光刻和电子束光刻等传统光刻技术制备,成本较高.寻找一种简单、低成本的纳米压印模板制备方法以提升纳米压印光刻技术的应用成为研究的重点与难点.本文以多孔氧化铝为母模板,采用纳米压印光刻技术对纳米多孔硅模板的制备进行了研究.在硅基表面成功制备出纳米多孔阵列结构,孔间距为350—560 nm,孔径在170—480 nm,孔深为200 nm.在激发波长为514 nm时,拉曼光谱的测试结果表明,相对于单面抛光的硅片,纳米多孔结构的硅模板拉曼光强有了约12倍左右的提升,对提升硅基光电器件的应用具有重要的意义.最后,利用多孔硅模板作为纳米压印母模板,通过热压印技术,成功制备出了聚合物纳米柱软模板.     

ZnO thin film on side polished optical fiber for gas sensing applications

In this work, thin ZnO films have been produced by pulsed laser deposition on side-polished fiber for optical gas sensor applications. The influence was investigated of the processing parameters, such as substrate temperature and oxygen pressure applied during deposition, on the sensitivity to ammonia of the sensing element. A shift of the spectral position of the resonance minimum to the longer wavelengths was observed at room temperature for the sample prepared at 150 °C substrate temperature and 20 Pa oxygen pressure. Spectral changes in the range 0.16-1.13 nm for NH₃ concentrations between 500 and 5000 ppm were also observed.     

Nanoparticles for dewetting suppression of thin polymer films used in chemical sensors

Addition of fullerenes (C₆₀ or buckyballs) to a linear polymer has been found to eliminate dewetting when a thin (∼50 nm) film is exposed to solvent vapor. Based on neutron reflectivity measurements, it is found that the fullerenes form a coherent layer approximately 2 nm thick at the substrate – polymer film interface during the spin-coating process. The thickness and relative fullerene concentration (∼29 vol%) is not altered during solvent vapor annealing and it is thought this layer forms a solid-like buffer shielding the adverse van der Waals forces promoted by the underlying substrate. Several polymer films produced by spin- or spray-coating were tested on both silicon wafers and live surface acoustic wave sensors demonstrating fullerenes stabilize many different polymer types, prepared by different procedures and on various surfaces. Further, the fullerenes drastically improve sensor performance since dewetted films produce a sensor that is effectively inoperable.     

新型酞菁的光致发光性质研究

研究了2,3-四-(2-异丙基一5-甲基苯氧基)氢酞菁在10,77,177和300 K下石英衬底上的浇铸膜和单晶硅衬底上真空镀膜(约200 nm厚)在300 K下光致发光光谱.氢酞菁的浇铸膜光致发光光谱在上述温度下均出现荧光发射和磷光发射峰,在177和300 K下出现了1 673 nm激基缔合物峰.该峰的出现与分子抗聚集能力的强弱有关,在300 K激基缔合物峰比在177 K下的峰强,从氢酞菁分子结构特点讨论了形成激基缔合物的原因.随着温度的升高,可以观察到荧光发射峰渐渐减弱而激基缔合物峰变强.由于浇铸膜和真空镀膜的酞菁分子聚集态不同导致了斯托克司位移的差异,真空镀膜的发光峰峰值在1 140 nm左右,与酞菁浇铸膜的峰值差别较大.浇铸膜的发光峰的半高宽为300 nm,而真空镀膜发光峰的半高宽为100 nm左右.     

Hydrogen permeation of tungsten phosphate glass thin films

Thin films of tungsten phosphate glasses were deposited on a Pd substrate by a pulsed laser deposition method and the flux of hydrogen passed thorough the glass film was measured with a conventional gas permeation technique in the temperature range 300–500 °C. The glass film deposited at low oxygen pressure was inappropriate for hydrogen permeation because of reduction of W ions due to oxygen deficiency. The membrane used in the hydrogen permeation experiment was a 3-layered membrane and consisted of Pd film (~ 20 nm), the glass film (≤ 300 nm) and the Pd substrate (250 µm). When the pressure difference of hydrogen and thickness of the glass layer were respectively 0.2 MPa and ~ 100 nm, the permeation rate through the membrane was 2.0 × 10^? 6 mol cm^? 2 s^? 1 at 500 °C. It was confirmed that the protonic and electronic mixed conducting glass thin film show high hydrogen permeation rate.     

表面等离子共振金/钯复合膜氢敏传感器

提出了一种新颖的钯(Pd)/金(Au)复合膜表面等离子共振氢敏结构,与单一Pd膜氢敏传感器相比,具有可靠性好、灵敏度高和响应度大等特点。利用表面等离子共振理论建立了Au/Pd复合膜氢敏传感器的数学模型,并对Au/Pd复合膜氢敏传感器的灵敏度进行了数值模拟。数值模拟结果表明:基于Au(2nm)/Pd(20nm)复合膜氢敏传感器所获得的最佳灵敏度比单一Pd(20nm)膜氢敏传感器提高了49 4%。     

Simple fabrication of hexagonally well-ordered AAO template on silicon substrate in two dimensions

In this study, thin anodic aluminum oxide (AAO) templates both on silicon substrates (AAO template/SiO₂/Si) and Ti-coated silicon substrates (AAO template/Ti/SiO₂/Si) were developed for design of magnetic, electronic and optoelectronic devices, chemical sensors and chip-scale lithium-ion rechargeable microbatteries. Two types of AAO template were prepared by using a two-step anodization procedure. The templates were characterized by scanning electron microscopy and energy dispersive X-ray spectroscopy. The obtained thin AAO templates were approximately 50 nm in diameter and 700 nm in length with 80-nm interpore distances in a relatively large area of 6 cm². A barrier layer of the AAO templates was removed by a cathodic polarization method in KCl solution for several seconds. The current–time transient during removing the alumina barrier layer of the thin AAO template and the mechanism of electrochemical dissolution of the barrier layer are given in detail.     

Nafion based amperometric hydrogen sensor

A Nafion based amperometric hydrogen sensor that operates at room temperature has been developed. The electrolyte used in the sensor is Nafion 117, which is a proton conducting solid polymer electrolyte. Palladium catalyst was used on the sensing side and platinum supported on carbon on the air side. The sensor functions as fuel cell, H₂/Pd//Nafion//Pt/O₂ and the short circuit current is measured. The short circuit current is found to be linear with respect to concentration of hydrogen on the sensing side. The sensor is able to detect the concentration of hydrogen in argon down to ppb level. Details of assembly of the sensor, response behavior and applications are discussed. Paper presented at the 2nd International Conference on Ionic Devices, Anna University, Chennai, India, Nov. 28–30, 2003.     

Sono-synthesis approach of reduced graphene oxide for ammonia vapour detection at room temperature

In this paper, we report the sono-synthesis of reduced graphene oxide (rGO) using polyethyleneimine (PEI), and its performance for ammonia vapour detection at room temperature. Graphene oxide (GO) and reduced graphene oxide (rGO) were prepared by sonication method by using low-frequency ultrasound under ambient condition and films were deposited by Doctor Blade method. The rGO, which has vapour accessible structure showed a good sensing response with a minimum detection limit of 1 ppm and the detection range from 1 ppm to 100 ppm. The sensing response was found to be 2% at 1 ppm and 34% at 100 ppm of ammonia and the developed sensor operated at room temperature. The sensor displays a response time of 6 s and a recovery time of 45 s towards 100 ppm of ammonia vapour. The source for the highly sensitive, selective and stable detection of ammonia with negligible interference from other vapours is discussed and reported. We believe reduced graphene oxide (rGO) could potentially be used to manufacture a new generation of low-power portable ammonia sensors.     

Novel optical film sensor design based on p-polarized reflectance

A new scheme of optical film sensor is presented. The sensor is based on p-polarized reflectance, consisting of a sensing coated substrate, is easily optimized for maximum sensitivity in different applications. The resolutions of refractive index n_f, extinction coefficient k_f and thickness h_f of the sensitive films are predicted to be 10⁻⁷, 10⁻⁵ and 10⁻³ nm, respectively. Experimentally, we selected the sol–gel derived SnO₂ films as gas-sensitive films and conducted preliminary gas-sensing test. The results indicate that novel optical film sensor scheme has higher sensitivity, and the detection sensitivity is available to 10⁻¹ ppm on the condition of optimum optical parameters and incident angle.     

Pd颗粒表面修饰ZnO纳米线阵列的制备及其气敏特性

采用化学气相沉积(CVD)方法在SiO_2/Si衬底生长了ZnO纳米线阵列,纳米线长约为15μm,直径为100~500 nm。通过改变溅射沉积时间(0~150 s),在ZnO纳米线表面包覆了不同厚度的Pd薄膜。在Ar气氛中,经800℃高温退火后,制备出Pd颗粒表面修饰的ZnO纳米线阵列并对其进行了气敏测试。对于乙醇而言,所有传感器最佳工作温度均为280℃。溅射时间的增加(3~10 s)导致ZnO纳米线表面Pd纳米颗粒数量及尺寸增加,传感器响应值由2.0增至3.6。过长的溅射时间(30~150 s)将导致Pd颗粒尺寸急剧增大甚至形成连续膜,传感器响应度显著降低。所有传感器对H2均表现出相对较好的选择性,传感器具有较好的响应-恢复特性和稳定性。最后,探讨了Pd颗粒表面修饰对ZnO纳米线阵列气敏传感器气敏特性的影响机制。     

Thickness dependent phase transformation of magnetron-sputtered Ni–Mn–Sn ferromagnetic shape memory alloy thin films

In this study, the influence of film thickness on the first-order martensite–austenite phase transformation of Ni–Mn–Sn ferromagnetic shape memory alloy thin films has been systematically investigated. Different thicknesses of the Ni–Mn–Sn films (from ~100 to 2,500 nm) were deposited by DC magnetron sputtering on Si (100) substrates at 550 °C. X-ray analysis reveals that all the films exhibit austenitic phase with the L2₁ cubic crystal structure at room temperature. The grain size and crystallization extent increase with the increase in film thickness, but the films with thickness above ~1,400 nm show structural deterioration due to the formation of MnSn₂ and Ni₃Sn₄ precipitates. The improvement in the crystallinity of the film with thickness is attributed to the decrease in film–substrate interfacial strain resulting in preferred oriented growth of the films. Temperature-dependent magnetization measurements as well as electrical measurements demonstrate the complete absence of phase transformation for the film of thickness of ~120 nm. For thickness greater than 400 nm, film exhibits the structural transformation, and it occurs at higher temperature with better hysteresis as film thickness is increased up to ~1,400 nm, after which degradation of phase transformation phenomenon is observed. This degradation is attributed to the disorders present in the films at higher thicknesses. Film with thickness ~1,400 nm possesses the highest magnetization with the smallest thermal hysteresis among all the films and therefore best suited for the actuators based on first-order structural phase transformation. Nanoindentation measurements reveal that the higher values of hardness and elastic modulus of about 5.5 and 215.0 GPa obtained in film of 1,014 nm thickness can considerably improve the ductility of ferromagnetic shape memory alloys (FSMA) and their applicability for MEMS applications. The exchange bias phenomenon is also found to be present in the films of thickness 1014, 1412, and 2022 nm exhibiting prominent martensitic transformation. Film of thickness 2,022 nm exhibits maximum exchange bias of ~50 Oe and higher exchange bias blocking temperature of 70 K as compared to other films.