Direct precipitation of silver nanoparticles induced by a high repetition femtosecond laser

Silver nanoparticles were precipitated directly in Ag⁺ doped silicate glass by a 150 fs, 800 nm, 250 kHz femtosecond laser irradiation. The irradiated pattern turned to yellow without heat treatment. The absorption peak about 400 nm, ascribed to the surface plasmon resonance of the formed silver nanoparticles, was observed. We believe that the reduced Ag atoms, via capturing free electrons created by multi-photon process, may aggregate into the Ag nanoparticles due to femtosecond laser inducing heat accumulation effect. This result has promising applications for the fabrication of 3D multi-colored images inside a transparent material.     

Formation of Si nanocrystals in glass by femtosecond laser micromachining

We report on the precipitation of Si nanocrystals inside a borosilicate glass by using an 800 nm, 250 kHz femtosecond laser irradiation, which was confirmed with X-ray diffraction, Raman spectra and transmission electron microscopy analyses. Refractive index profile reveals that the refractive index of the Si nanocrystals precipitated region increased up to 8.7% in comparison with that of the unirradiated area, leading to a large diffraction efficiency of the fabricated dot structure. Furthermore, the third-order optical nonlinearity of the Si nanocrystals precipitated glass is greatly enhanced based on the Z-scan measurement. These results may find applications for the fabrication diffractive optical devices and optical switches.     

飞秒激光诱导玻璃内Ba2TiSi2O8晶体的析出

使用聚焦后的800nm,150fs,250kHz的高重复频率飞秒脉冲激光器能够在BaO-TiO₂-SiO₂组分的玻璃内部三维选择性地诱导Ba₂TiSi₂O₈晶体的析出. 发光光谱显示这种晶体把入射的800nm光转化成了400nm的蓝光,因此这种析出的晶体具有非线性倍频特性. 通过拉曼光谱测定,在当前的玻璃组分中析出的晶体是Ba₂TiSi₂O₈. 研究表明,经250kHz的飞秒激光辐照一段时间后,在玻璃内部由于脉冲能量的连续沉积会使得激光辐照区域出现热积累效应,因此,该辐照区域的温度会不断升高以致超过玻璃析晶温度,最终诱导玻璃熔融析晶. 此外,对飞秒激光辐照区域不同部位进行拉曼光谱检测,结果表明：在整个区域Ba₂TiSi₂O₈晶体的析出呈现中间比外围明显的分布特点,因此晶体析出与辐照形成的温度梯度场有密切关系.     

Application of femtosecond-laser induced nanostructures in optical memory

The femtosecond laser induced micro- and nanostructures for the application to the three-dimensional optical data storage are investigated. We have observed the increase of refractive index due to local densification and atomic defect generation, and demonstrated the real time observation of photothermal effect after the femtosecond laser irradiation inside a glass by the transient lens (TrL) method. The TrL signal showed a damped oscillation with about an 800 ps period. The essential feature of the oscillation can be reproduced by the pressure wave creation and propagation to the outward direction from the irradiated region. The simulation based on elastodynamics has shown that a large thermoelastic stress is relaxed by the generation of the pressure wave. In the case of soda-lime glass, the velocity of the pressure wave is almost same as the longitudinal sound velocity at room temperature (5.8 microm/ns). We have also observed the localized photo-reduction of Sm3+ to Sm2+ inside a transparent and colorless Sm(3+)-doped borate glass. Photoluminescence spectra showed that some the Sm3+ ions in the focal spot within the glass sample were reduced to Sm2+ ions after femtosecond laser irradiation. A photo-reduction bit of 200 nm in three-dimensions can be recorded with a femtosecond laser and readout clearly by detecting the fluorescence excited by Ar+ laser (lambda = 488 nm). A photo-reduction bit can be also erased by photo-oxidation with a cw Ar+ laser (lambda = 514.5 nm). Since photo-reduction bits can be spaced 150 nm apart in a layer within glass, a memory capacity of as high as 1 Tbit can be achieved in a glass piece with dimensions of 10 mm x 10 mm x 1 mm. We have also demonstrated the first observation of the polarization-dependent periodic nanostructure formation by the interference between femtosecond laser light and electron acoustic waves. The observed nanostructures are the smallest embedded structures ever created by light. The period of self-organized nanostructures can be controlled from approximately 140 to 320 nm by the pulse energy and the number of irradiated pulses. Furthermore, we have also observed the self-assembled sub-wavelength periodic structures created in silica glass by femtosecond pulses on the plane of the propagation of light.     

Effect of ion irradiation on internal stress of amorphic carbon films produced by pulsed laser

Amorphic carbon films either 50 or 160 nm thick were deposited on Si(100) and glass substrates at room temperature in a high-vacuum environment using a Q-switched Nd-YAG pulse laser focused on a graphite target. These films were irradiated with Ti⁺ or C⁺ ions having kinetic energies of 35 and 75 keV, and the changes in internal stresses of the films with varying ion influence were investigated by measuring substrate bending using stylus profilometry. The ion energy and the film thickness were chosen such that the ion penetration depth, R_p, corresponded to either the film thickness or one half of the film thickness. The results indicate that there is an optimum ion fluence leading to a stress-free film for a given ion species and energy. Interpretation of the resulting stress behavior from ion irradiation was made based on the relaxation resulting from damage inside the film together with interfacial mixing. The scanning electron microscopy pictures and surface roughness measurements showed a very smooth surface for both as-deposited and ion-irradiated films. The ion-irradiated films had a Vickers hardness greater than 22 GPa, and were adherent to both Si and glass substrates. An investigation of the film characteristics using Raman scattering and electron-energy loss spectra has revealed that high-energy ion irradiation of an intermediate ion fluence can be utilized successfully to deposit an adherent and hard carbon film with controlled internal stress without changing the film structure significantly.     

Effect of the thickness of Si film on Si/Se film doped silicon prepared by femtosecond laser

The high infrared absorption of silicon could be achieved by doping silicon with chalcogens via femtosecond laser. In the paper, the samples of Se-doped silicon with different thickness of Si film were prepared with the aid of femtosecond laser. The effect of the thickness of silicon film on optical and the electrical properties of se-doped silicon is investigated. All the samples were thermally annealed at 500 °C for 1 h, and the absorptance of all the samples was found with a certain degree of reduction. With the increase of thickness of silicon film, the results of visible-near infrared spectrum showed that the infrared absorptance increased first and then decreased. In particular, the optical absorption, sheet carrier density and responsivity for samples prepared with the silicon film that was 300 nm thick were greater than that of the samples prepared with the Si films of other thickness. The experiment demonstrated that it is significant to select the silicon film of appropriate thickness in the fabrication of Se doped silicon.     

新型三明治结构铝诱导非晶硅薄膜低温晶化增强

本文对比探索了新型Al/α -Si/Al三明治结构与传统的Al/α -Si双层结构对铝诱导非晶硅薄膜低温晶化结果的影响,结果表明在相同的制备及退火条件下,前者更利于形成高度晶化的多晶硅薄 .膜.本研究工作利用拉曼光谱、掠入射X射线衍射、光学显微镜、方块电阻等表征方法探讨了薄膜厚度比和退火温度对金属诱导非晶硅薄膜晶化的程度、晶体结构以及电学性能的影响,最终制备出了电阻率仅为2.5 Ω·cm的多晶硅薄膜.     

Growth mechanism of Si nodules on BPSG

Si nodules that appear in the metal electrodes of integrated circuits often reduce their reliability. The growth process of Si nodules generated on boro-phospho silicate glass (BPSG) in the Al-1 wt.% Si film electrode has been investigated. The Al-1 wt.% Si films sputter deposited on BPSG films were annealed at 723 K for 30 min according to the usual integrated circuit procedure. Scanning electron microscopy and atomic force microscopy observations revealed that the Si nodules seemed to precipitate along Al grain boundaries particularly on the BPSG film and their shape appeared pyramidal. To make clear the mechanism of the growth of the Si nodule on the BPSG film, the interface between the Si nodule and the BPSG film was investigated in detail by transmission electron microscopy, electron diffraction and energy dispersive X-ray spectroscopy. As the result, it was found that there existed an amorphous silicon oxide region in the central part of the interface under the Si nodule. The amorphous silicon oxide is considered to be formed by diffusion of oxygen from the BPSG film to the Si nodule during the annealing. The amorphous silicon oxide may act as an embryo for the formation of the Si nodule and the migration of Si atoms dissolved in Al towards the embryo seems to enhance the growth of the Si nodule.     

Investigation of the aluminum oxide/Si(1 0 0) interface formed by chemical vapor deposition

Thin films of aluminum oxide were deposited using trimethylaluminum and oxygen. The deposition rate was found to decrease with increasing temperature. Fourier transform infrared spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to investigate the film/substrate interface. When dry O₂ was used during deposition, the film/substrate interface was free of any silicon dioxide or aluminum silicate phase. On annealing the as-deposited films in Ar, a layer of silicon dioxide film formed at the interface. XPS results indicated that the O/Al ratio in the as-deposited films was higher than that in stoichiometric Al₂O₃. However, the ratio was found to decrease in the annealed samples suggesting that excess oxygen present in the deposited films is responsible for the formation of interfacial silicon dioxide layer. Interfacial phase formation was observed in the as-deposited samples, when small amounts of ozone along with oxygen were used as the oxygen precursor.     

Effect of the initial structure on the electrical property of crystalline silicon films deposited on glass by hot-wire chemical vapor deposition

Crystalline silicon films on an inexpensive glass substrate are currently prepared by depositing an amorphous silicon film and then crystallizing it by excimer laser annealing, rapid thermal annealing, or metal-induced crystallization because crystalline silicon films cannot be directly deposited on glass at a low temperature. It was recently shown that by adding HCI gas in the hot-wire chemical vapor deposition (HWCVD) process, the crystalline silicon film can be directly deposited on a glass substrate without additional annealing. The electrical properties of silicon films prepared using a gas mixture of SiH4 and HCl in the HWCVD process could be further improved by controlling the initial structure, which was achieved by adjusting the delay time in deposition. The size of the silicon particles in the initial structure increased with increasing delay time, which increased the mobility and decreased the resistivity of the deposited films. The 0 and 5 min delay times produced the silicon particle sizes of approximately 10 and approximately 28 nm, respectively, in the initial microstructure, which produced the final films, after deposition for 300 sec, of resistivities of 0.32 and 0.13 Omega-cm, mobilities of 1.06 and 1.48 cm2 V(-1) S(-1), and relative densities of 0.87 and 0.92, respectively.     

Crystallization of amorphous hydrogenated silicon (<Emphasis Type="Italic">a</Emphasis>-Si:H) films under irradiation with femtosecond laser pulses

Crystallization of thin films of amorphous hydrogenated silicon under the irradiation of femtosecond laser pulses has been studied. It was found that the crystallization has a clearly pronounced threshold nature and depends on the laser emission wavelength. As shown the best results are achieved in crystallization at the laser wavelength range of 740–760 nm.     

Aluminum-induced in situ crystallization of HWCVD a-Si:H films

Aluminum-induced in situ crystallization (AIC) of amorphous silicon films deposited by hot wire chemical vapor deposition (HWCVD) on glass is demonstrated. Aluminum was deposited at temperatures varying from room temperature to 300 °C on HWCVD a-Si:H films. The AIC was observed to take place in situ during the deposition of Al films, when the glass/a-Si:H temperature is kept 300 °C. A 20-nm Al film was effective in inducing crystallization of about 63% in the a-Si:H film. Thus, separate post-deposition annealing step can be avoided. For an Al film thickness comparable to the amorphous silicon film deposited at an optimum deposition rate, crystallization at temperature as low as 200 °C is observed. It was also observed that the growth pattern of c-Si in case of AIC without post-deposition annealing was identical to AIC with annealing step.     

Temperature dependence of the stress in PSG/AlSi structures

The temperature dependence of the stress in each layer of a film system comprising chemically vapour-deposited phosphosilicate glass (PSG) on an AlSi alloy film on a silicon substrate was investigated in the range 20–500°C. During a heating process in which the temperature exceeded 150°C, the deformation of the AlSi film was found to be caused by diffusional creep, and the stresses in both the AlSi film and the PSG film increased with increasing silicon concentration in the AlSi film. Deformation of AlSi film during a cooling process in which temperatures were higher than 150°C was found to be caused by the generation of dislocation loops or by grain boundary sliding. These phenomena are interpreted as representing relaxation of the total elastic energy of the system which results from the deformation of the AlSi film.     

The nanoporous structure of anodic aluminum oxide fabricated on the Au/Nb/Si substrate

We have studied the anodization behavior of an Al film evaporated on the Au/Nb/Si substrate and demonstrated an effective approach to fabricate the through-hole anodic aluminum oxide (AAO) template on the conducting substrate. The smoothness of the initial metal films and an appropriate wet etching of the oxide film anodized in the first step were found to be critical factors for successfully anodizing the Al film on Au surface. The barrier layer of the obtained AAO structure presented a convex and thinner characteristic, and the underlying Au surface became porous after the anodization. This phenomenon was similar to the case of anodizing the Al film on an ITO glass substrate and could be explained reasonably by the effect of high pressure O₂ gas impelling and H⁺ etching at the interface of the barrier oxide and the Au layer.     

准分子激光引起的非晶硅薄膜晶化行为的研究

利用KrF准分子激光对非晶硅薄膜的表层进行了晶化.研究了激光能量密度和照射脉冲数对薄膜结晶度的影响,并对晶化后薄膜的形貌和结构进行了表征.结果表明:该非晶硅薄膜晶化阈值约为110 mJ/cm2,且不受照射脉冲数的影响;激光能量密度是影响薄膜结晶度的首要因素,但在较低的能量密度时,增加照射脉冲数也会显著的提高薄膜结晶度;结构及形貌表征发现,薄膜晶化层厚度约为400～500 nm,平均晶粒尺寸为30～50 nm.     

Mechanisms of pulsed laser microbeam release of SU-8 polymer "micropallets" for the collection and separation of adherent cells

The release of individual polymer micropallets from glass substrates using highly focused laser pulses has been demonstrated for the efficient separation, collection, and expansion of single, adherent cells from a heterogeneous cell population. Here, we use fast-frame photography to examine the mechanism and dynamics of micropallet release produced by pulsed laser microbeam irradiation at lambda = 532 nm using pulse durations ranging between 240 ps and 6 ns. The time-resolved images show the laser microbeam irradiation to result in plasma formation at the interface between the glass coverslip and the polymer micropallet. The plasma formation results in the emission of a shock wave and the ablation of material within the focal volume. Ablation products are generated at high pressure due to the confinement offered by the polymer adhesion to the glass substrate. The ablation products expand underneath the micropallet on a time scale of several hundred nanoseconds. This expansion disrupts the polymer-glass interface and accomplishes the release of the pallet from its glass substrate on the microsecond time scale (approximately 1.5 micros). Our experimental investigation demonstrates that the threshold energy for pallet release is constant (approximately 2 microJ) over a 25-fold range of pulse duration spanning the picosecond to nanosecond domain. Taken together, these results implicate that pallet release accomplished via pulsed laser microbeam irradiation is an energy-driven plasma-mediated ablation process.     

Formation of void array inside transparent and absorptive glasses by femtosecond laser irradiation

We demonstrate self-fabrication of void arrays in a fused silica transparent in the visible and a color-filter borosilicate glass strongly absorptive at 800 nm using tightly focused Ti-sapphire femtosecond laser pulses at 1 kHz without scanning. The period, the size, the number of voids, and the length of the aligned void structure were controlled by changing the laser pulse energy, and the position of the focal point inside two materials. The void arrays were observed by an optical microscope and also estimated by an optical diffraction experiment. The void size and period were smaller in the absorptive glass than in the transparent glass. The submicrometer-sized void was observed by a scanning electron microscope. The smaller and clearer void arrays were formed in the color filter than the fused silica glass. With increasing the laser focal depth, the void-array length increased in the fused silica and decreased in the color filter.     

Fabrication of diffractive optical elements inside polymers by femtosecond laser irradiation

Bragg-type gratings were prepared by irradiation inside a series of optical polymers with femtosecond laser pulses and the preparation conditions of the grating were examined. Repeated scanning irradiation with femtosecond laser pulses formed gratings due to refractive index changes inside polymers. Among the polymers examined in the present study, polymethylpentene (PMP) showed the highest diffraction efficiency, which was an order of magnitude higher than those of other optical polymers. The density of PMP was the lowest among the polymers evaluated in the present study, and the large volume contraction based on its low density was responsible for the larger refractive index change of PMP. Furthermore, we fabricated large-area diffractive optical elements (DOEs) in PMP measuring 15 × 25 mm² by widening the scanning area.     

Development and Mechanical Behavior of FML/Aluminium Foam Sandwiches

In this study, the Fiber-Metal Laminates (FMLs) containing glass fiber reinforced polypropylene (GFPP) and aluminum (Al) sheet were consolidated with Al foam cores for preparing the sandwich panels. The aim of this article is the comparison of the flexural properties of FML/Al foam sandwich panels bonded with various surface modification approaches (silane treatment and combination of silane treatment with polypropylene (PP) based film addition). The FML/foam sandwich systems were fabricated by laminating the components in a mould at 200 °C under 1.5 MPa pressure. The energy absorbtion capacities and flexural mechanical properties of the prepared sandwich systems were evaluated by mechanical tests. Experiments were performed on samples of varying foam thicknesses (8, 20 and 30 mm). The bonding among the sandwich components were achieved by various surface modification techniques. The Al sheet/Al foam sandwiches were also consolidated by bonding the components with an epoxy adhesive to reveal the effect of GFPP on the flexural performance of the sandwich structures.     

带有力反馈控制的三明治式微机械干涉加速度计

设计了一种静电力反馈控制的三明治式微机械干涉加速度计,加速度计由敏感芯片、半导体激光器、光电二极管以及相应的驱动电路和反馈控制电路组成.敏感芯片为玻璃-硅-玻璃3层结构,通过硅-玻璃键合体硅工艺制成.硅质量块由铝梁支撑,底部玻璃基片上有金属光栅和电极,通过在质量块和底部玻璃基片上的电极之间施加电压可以调节质量块与玻璃基片间的间隙.入射激光照射到敏感芯片上的光栅上,产生衍射光束,其光强随质量块与下玻璃的间距而变化.反馈控制电路通过测量衍射光强的变化来改变质量块与底电极之间的电压,使得质量块与底部玻璃基片的距离保持为入射光波长1/8的奇数倍,从而提高输出线性度,改善灵敏度,增大量程.