Influence of different substrates on laser induced damage thresholds at 1064 nm of Ta2O5 films

Ta2O5 films are prepared on Si, BK7, fused silica, antireflection (AR) and high reflector (HR) substrates by electron beam evaporation method, respectively. Both the optical property and laser induced damage thresholds (LIDTs) at 1064 nm of Ta2O5 films on different substrates are investigated before and after annealing at 673 K for 12h. It is shown that annealing increases the refractive index and decreases the extinction index, and improves the O/Ta ratio of the Ta2O5 films from 2.42 to 2.50. Moreover, the results show that the LIDTs of the Ta2O5 films are mainly correlated with three parameters: substrate property, substoichiometry defect in the films and impurity defect at the interface between the substrate and the films. Details of the laser induced damage models in different cases are discussed.

Laser induced damage threshold at 355 and 1064 nm of Ta2O5 films of different phases

Ta2O5 films are deposited on fused silica substrates by conventional electron beam evaporation method. By annealing at different temperatures, Ta2O5 films of amorphous, hexagonal and orthorhombic phases are obtained and confirmed by x-ray diffractometer ( XRD) results. X-ray photoelectron spectroscopy ( XPS) analysis shows that chemical composition of all the films is stoichiometry. It is found that the amorphous Ta2O5 film achieves the highest laser induced damage threshold ( LIDT) either at 355 or 1064 nm, followed by hexagonal phase and finally orthorhombic phase. The damage morphologies at 355 and 1064 nm are different as the former shows a uniform fused area while the latter is centred on one or more defect points, which is induced by different damage mechanisms. The decrease of the LIDT at 1064nm is attributed to the increasing structural defect, while at 355nm is due to the combination effect of the increasing structural defect and decreasing band gap energy.

不同方法制备的Ta_2O_5薄膜光学性能和激光损伤阈值的对比分析

采用电子束蒸发(EBE)和离子束溅射(IBS)制备了不同的Ta_2O_5薄膜,同时对电子束蒸发制备的薄膜进行了退火处理。研究了制备的Ta_2O_5薄膜的光学性能、激光损伤阈值(LIDT)、吸收、散射、粗糙度、微缺陷密度和杂质含量。结果表明,退火可使电子束蒸发制备的薄膜的光学性能得到改善,接近离子束溅射的薄膜的光学性能。电子束蒸发制备的薄膜的损伤阈值较低的主要原因在于吸收大,微缺陷密度和杂质含量高,而与薄膜的散射和粗糙度关系不大。退火后薄膜的吸收和微缺陷密度都明显降低,损伤阈值得到提高。退火后的薄膜损伤阈值仍然低于溅射得到的薄膜损伤阈值是因为退火并不能降低膜内的杂质含量,因此选用高纯度的蒸发膜料和减少电子束蒸发过程中的污染有可能进一步提高薄膜的损伤阈值。

355nm增透膜的设计、制备与性能

用热舟蒸发法结合修正挡板技术制备了355 nm LaF3/MgF2增透膜,并对部分样品进行了真空退火。采用Lambda 900光谱仪测试了增透膜的低反光谱和透射光谱,并考察了其光谱稳定性;使用脉冲8 ns的355 nm激光测试了增透膜的激光损伤阈值(LIDT);采用Normarski显微镜对增透膜的表面缺陷密度和破斑形貌进行了观察。实验结果表明,制备得到的增透膜的剩余反射率较低,光谱稳定性好;真空退火对增透膜的激光损伤阈值没有改善;增透膜的破环形貌为散点形式,结合破斑深度测试表明薄膜的破坏源于薄膜和基底界面的缺陷点。JGS1熔石英基底由于有好的表面状况、固有的高激光损伤阈值和以其为基底的增透膜具有更低的表面场强,使得其上的增透膜有更高的抗激光损伤能力。

Influence of laser preconditioning on the capacity of optical films to resist laser-induced damage

As a technique to improve the ability of optical films to resist laser-induced damage (ARLID), laser preconditioning has been investigated broadly. In this paper, the laser preconditioning effect has been analyzed based on the defect-initialized damage mechanism that the author had put forward previously. Theoretical results show that an energy density scope (PEDS) exists in which the preconditioning laser can effectively improve the ARLID of optical films. In addition, when the energy density of the testing laser pulse is altered, the boundary of PEDS will change accordingly. Experimental results have verified these theoretical assumptions. PEDS will also become wider if the critical energy density of the preconditioning laser that can induce films' micro-damage increases, or the critical energy density of the preconditioning laser that can cause laser annealing decreases. In these cases, it is relatively easy to improve the ARLID of optical films. Results of the current work show great significance in enhancing the ARLID of optical films through the laser preconditioning technique. (C) 2008 Elsevier B.V. All rights reserved.

Influence of substoichiometer on the laser-induced damage characters of HfO2 thin films

HfO2 is one of the most important high refractive index materials for depositing high power optical mirrors. In this research, HfO2 thin films were prepared by dual-ion beam reactive sputtering method, and the laser-induced damage thresholds (LIDT) of the sample were measured in 1-on-1 mode for laser with 1064 nm wavelength. The results indicate that the LIDT of the as-grown sample is only 3.96 J/cm(2), but it is increased to 8.98 J/cm(2) after annealing under temperature of 200 degrees C in atmosphere. By measuring the laser weak absorption and SIMS of the samples, we deduced that substoichiometer is the main reason for the low LIDT of the as-grown sample, and the experiment results were well explained with the theory of electronic-avalanche ionization. (C) 2008 Elsevier B.V. All rights reserved.

Investigation on thermal stability of TiO2 films for application at high temperature

The thermal stability of electron beam deposited TiO2 monolayers and TiO2/SiO2 high reflectors (HR) during 300 to 1100 degrees C annealing is studied. It is found that the optical loss of film increases with the increase in annealing temperature, due to the phase change, crystallisation and deoxidising of film. Scattering loss dominates the optical property degradation of film below 900 degrees C, while the absorption is another factor at 1100 degrees C. The increase in refractive index and decrease in physical thickness of TiO2 layer shift the spectra of HR above 900 degrees C. The possible crack mechanism on the surface of HR during annealing is discussed. Guidance for application on high temperature stable optical coatings is given.

High refractive index TiO2 film deposited by electron beam evaporation

The well known 'crystal seed' theory is first applied in this work to prepare TiO2 film: a high refractive index rutile TiO2 film is grown by electron beam evaporation on the rutile seed formed by 1100 degrees C annealing. The average n is larger than 2.4, by far the highest in all the authors' TiO2 films. The films are characterised by optical properties, microstructure and surface morphologies. It is found that the refractive index shows positive relation with the crystal structure, grain size, and packing density and roughness of the film. The film has lower density of granularity and nodule defects on the surface than those of the film deposited by magnetron sputtering. The result shows attractive application in complex filter and laser coatings.

Síntese e caracterização de TiO2 puro e modificado para aplicações ambientais

Fotocatalisadores baseados em nanopartículas de dióxido de titânio modificados fornecem soluções em potencial para a mineralização de poluentes orgânicos em meio aquoso. Agentes modificadores têm sido amplamente investigados com o objetivo de promover a fotoativação pela luz visível. Foram estudadas a nível fundamental até aqui, as modificações estruturais, texturais e óticas causadas pela introdução de silício e nitrogênio na rede da titânia. Titânias puras (TiO2) e modificadas nanoestruturadas, particularmente titânias modificadas com silício (TiO2-SiO2), com razões atômicas Si/Ti de 0,1, 0,2 e 0,3 foram sintetizadas pelo método sol-gel a partir da hidrólise ácida de isopropóxido de titânio(IV) e tetraetoxisilano. As metodolo-gias sintéticas desenvolvidas tentaram aderir aos princípios da Química Verde, dispensando o uso de atmosfera inerte e temperatura e pressão elevadas, o que foi alcançado utilizando-se, principalmente, a agitação ultrassônica. Titânias modificadas com silício e dopadas com ni-trogênio (TiO2-SiO2-N) foram obtidas a partir do pré-tratamento de TiO2-SiO2 a 500 C ao ar e então submetidas ao fluxo de amônia (NH3) a 600 C por 1-3 h e, após resfriamento, foram recozidas a 400 C ao ar. Amostras distintas foram caracterizadas, na forma de pó seco e após calcinação entre 400600 C, por difração de raios X, adsorção de nitrogênio, microscopia eletrônica de varredura e espectroscopia de refletância difusa no UV-Visível. As titânias pu-ras, obtidas principalmente variando-se a razão de hidrólise, foram cristalizadas na forma de anatásio como fase predominante até 600 C, além de traços de brookita presente até 500 C. O rutilo foi identificado a partir de 600 C como fase minoritária, embora apresentando tama-nhos de cristal significativamente maiores que os estimados para o cristal de anatásio. As titâ-nias modificadas com até 20% de silício apresentaram notável estabilidade térmica, evidenci-ada pela presença exclusiva de anatásio até 900 C. Foi também observado o aparecimento de macroporos com diâmetro médio em torno de 55 nm após calcinação a 400 C, diferentemente do que se observou nas amostras em geral. A introdução de baixo teor de silício assegurou às titânias calcinadas valores elevados de área específica, atribuído ao efeito de contenção acentuada na taxa de crescimento do cristal. As titânias modificadas com silício e as titânias puras obtidas com taxa de hidrólise 25:1 para a razão H2O : Ti apresentaram mesoporos com diâmetros médios de mesma dimensão do cristal. As titânias modificadas com silício e dopa-das com nitrogênio apresentaram absorção na região visível entre 400-480 nm, com discreta redução da energia de band gap para as transições eletrônicas consideradas. Titânias calcina-das a 300−400 C apresentaram desempenho fotocatalítico semelhante ao TiO2 P25 da De-gussa sob irradiação UV, na degradação do azo corante Reactive Yellow 145 em soluções a-quosas em pH 5 a 20 1C

Nonvolatile memory functionality of ZnO nanowire transistors controlled by mobile protons.

We demonstrated the nonvolatile memory functionality of ZnO nanowire field effect transistors (FETs) using mobile protons that are generated by high-pressure hydrogen annealing (HPHA) at relatively low temperature (400 °C). These ZnO nanowire devices exhibited reproducible hysteresis, reversible switching, and nonvolatile memory behaviors in comparison with those of the conventional FET devices. We show that the memory characteristics are attributed to the movement of protons between the Si/SiO(2) interface and the SiO(2)/ZnO nanowire interface by the applied gate electric field. The memory mechanism is explained in terms of the tuning of interface properties, such as effective electric field, surface charge density, and surface barrier potential due to the movement of protons in the SiO(2) layer, consistent with the UV photoresponse characteristics of nanowire memory devices. Our study will further provide a useful route of creating memory functionality and incorporating proton-based storage elements onto a modified CMOS platform for FET memory devices using nanomaterials.

Spontaneous formation of highly ordered nanostructures: thermal instability and mode selection in surface-capped polymer films.

We demonstrate a controllable formation process of wave-like patterns in thermally unstable surface-capped polymer films on a rigid substrate. Self-ordered wave-like structures over a large area can be created by applying a small lateral tension to the film, whereupon it becomes unstable. A clear mode selection process which includes creation, decay and interference between coexisting waves at different annealing conditions has been observed, which makes it possible to restrain the patterns which are formed finally. Our results provide a clear and new evidence of spinodal behaviour in such a film due to thermal instability. Furthermore, we show that the well-controlled patterns generated in such a process can be used to fabricate nanostructures for various applications.

Tubular graphite cones with single-crystal nanotips and their antioxygenic properties.

Tubular graphite cones (TGCs) with a single-crystal nanotip have been achieved by means of microwave plasma-assisted chemical vapor deposition using in-situ-evaporated Fe catalysts. The absence of the disorder-induced D band in Raman spectra revealed the single-crystalline feature of the nanotip. TGCs were found to stem from Fe catalytic carbon spherules on the order of 100 mum diameter, whose critical role in promoting both nucleation and plasma annealing in the formation of highly crystalline TGCs is discussed. The crystalline quality of such TGCs can be further verified by the investigation of their oxidative stability in air. All TGCs can survive up to 600 degrees C without any structural variations, and a few TGCs still survive with an anisotropic etched and stepped nanotip at temperatures up to 800 degrees C, much better than CNTs. Thus, TGCs with single crystalline nanotips are potential candidates for scanning probes in high-temperature oxygen-containing environments.

Growth of carbon nanotubes on fully processed silicon-on-insulator CMOS substrates.

This paper describes the growth of Carbon Nanotubes (CNTs) both aligned and non-aligned on fully processed CMOS substrates containing high temperature tungsten metallization. While the growth method has been demonstrated in fabricating CNT gas sensitive layers for high temperatures SOI CMOS sensors, it can be employed in a variety of applications which require the use of CNTs or other nanomaterials with CMOS electronics. In our experiments we have grown CNTs both on SOI CMOS substrates and SOI CMOS microhotplates (suspended on membranes formed by post-CMOS deep RIE etching). The fully processed SOI substrates contain CMOS devices and circuits and additionally, some wafers contained high current LDMOSFETs and bipolar structures such as Lateral Insulated Gate Bipolar Transistors. All these devices were used as test structures to investigate the effect of additional post-CMOS processing such as CNT growth, membrane formation, high temperature annealing, etc. Electrical characterisation of the devices with CNTs were performed along with SEM and Raman spectroscopy. The CNTs were grown both at low and high temperatures, the former being compatible with Aluminium metallization while the latter being possible through the use of the high temperature CMOS metallization (Tungsten). In both cases we have found that there is no change in the electrical behaviour of the CMOS devices, circuits or the high current devices. A slight degradation of the thermal performance of the CMOS microhotplates was observed due to the extra heat dissipation path created by the CNT layers, but this is expected as CNTs exhibit a high thermal conductance. In addition we also observed that in the case of high temperature CNT growth a slight degradation in the manufacturing yield was observed. This is especially the case where large area membranes with a diameter in excess of 500 microns are used.

Effect of deposition conditions on the chemical bonding in sputtered carbon nitride films

A balanced planar r.f. powered magnetron sputter source has been used to deposit carbon nitride films from a graphite target under various conditions. Sample temperature, bias voltage and nitrogen content in the gas mixture were varied. The effects of oxygen, methane and ammonia on the film growth were also studied. Special attention was paid to the effects of the deposition parameters on the structure of the films, in particular the hybridisation of the carbon and nitrogen bonding. The chemical bonding of the carbon and nitrogen atoms was studied by electron energy loss spectroscopy (EELS). The chemical composition was evaluated by Rutherford back-scattering. The intensity of transitions to π antibonding orbitals, as revealed by EELS, was found to increase with the nitrogen content in the films. Ion bombardment of the films during growth and the addition of oxygen or hydrogen-rich gases further increased the proportion of π bonds of both the carbon and nitrogen atoms. It is suggested that the increase in the transitions to μ antibond orbitals is to be explained by increased sp2 or possibly sp hybridisation of the carbon and nitrogen. Also, the effect of annealing on the bonding of nitrogen rich films after deposition was tested. The changes caused by nitrogen and deposition conditions are consistent with previous reports on the formation of paracyanogen structures.

Application of electron beams in thermal processing of semiconductor materials and devices

Rapid and effective thermal processing methods using electron beams are described in this paper. Heating times ranging from a fraction of a second to several seconds and temperatures up to 1400°C are attainable. Applications such as the annealing of ion implanted material, both without significant dopant diffusion and with highly controlled diffusion of impurities, are described. The technique has been used successfully to activate source/drain regions for fine geometry NMOS transistors. It is shown that electron beams can produce localised heating of semiconductor substrates and a resolution of approximately 1 μm has been achieved. Electron beam heating has been applied to improving the crystalline quality of silicon-on sapphire used in CMOS device fabrication. Silicon layers with defect levels approaching bulk material have been obtained. Finally, the combination of isothermal and selective annealing is shown to have application in recrystallisation of polysilicon films on an insulating layer. The approach provides the opportunity of producing a silicon-on-insulator substrate with improved crystalline quality compared to silicon-on-sapphire at a potentially lower cost. It is suggested that rapid heating methods are expected to provide a real alternative to conventional furnace processing of semiconductor devices in the development of fabrication technology. © 1984 Benn electronics Publications Ltd, Luton.