用于XeF蓝绿激光器的表面放电光泵浦源

基于Al2O3陶瓷、BN陶瓷和聚四氟乙烯三种基底建立了分段表面放电光泵浦源,对比研究了这三种表面放电光泵浦源的电学特性、辐射特性和烧蚀特性。利用放电波形计算了表面放电光泵浦源的等效电感、等效电阻和沉积效率,应用光谱法比较了它们的紫外辐射强度,并采用平均线烧蚀率评估了三种泵浦源的耐烧蚀性能。通过比较研究发现,在充电电压为13.5~26.8kV、间隙长度为8cm、放电室内混合气体气压为100kPa条件下,三种泵浦源中Al2O3陶瓷表面放电光泵浦源的沉积效率最高,大于82%;辐射光谱具有紫外增强效应,紫外辐射最强;平均线烧蚀率最小(小于0.15μm/shot),耐烧蚀性能最好。研究结果表明采用Al2O3陶瓷表面放电光泵浦源作为大功率重频XeF蓝绿激光器的泵浦源,可提高XeF蓝绿激光器的寿命。     

Analysis of surface and material modifications caused by laser drilling of AlN ceramics

For the laser drilling of aluminum nitride ceramic the processing results and the effects related to pulsed irradiation were investigated. Images of the drilled surface revealed regular, cylindrically shaped holes of about 100 μm in diameter independently of the laser wavelength (1064/532/355 or 266 nm). The holes were surrounded by circular heat-affected zones of larger diameter. A comparison of the elemental compositions of the original material and the processed one indicated a decrease of the nitrogen concentration in the affected area. The spectral analysis of the ablated material composition revealed the presence of ions and neutrals in dependence on the laser intensity applied. It was found that at intensity values close to the ablation threshold the ejected material consisted mainly of neutrals, while doubling of the intensity resulted in appearance of single-ionized Al species, which were also observed together with Al clusters in the mass spectra of the UV-excited plasma. Their prevailing content was revealed for drilling at higher intensities around 15 GW/cm² at 532 nm. Results of model calculations indicated, in agreement with the experiment, that at the threshold the ceramic decomposes into gaseous nitrogen and solid Al particulates, while at a higher fluence the material particles vaporize and influence the quality of drilling.     

Polymer‐filler derived ceramics with low shrinkage using PCS/SiC/Al mixture

Active Al and inert SiC powders were dispersed in the polycarbosilane to manufacture SiC ceramic composites by a new process of active‐filler‐controlled pyrolysis of polymer. 40 wt% of active Al fillers, 40 wt% of inert SiC fillers and 20 wt% of PCS, were homogenized. The samples were obtained by pyrolysis at 1100 °C for different soaking time. The results showed that due to the incorporation of active Al fillers, formation of crystallite phases such as Al₄C₃, Al₄Si₃ and AlN occured due to the of reaction of Al particles with the polymer decomposition products and the reactive nitrogen atmosphere. The microstructural and mechanical characterization results of the composites are presented in the paper. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Modelling of laser surface alloying and dispersing of ceramics

Laser‐supported processes can be used to modify the electrical and thermal properties of ceramic substrates locally. These processes are characterized by a strong thermal interaction between the laser beam and the ceramic surface that leads to localized melting. During the dynamic melting process an additive material is injected into the melt pool in order to modify the physical properties. The heat and mass transfer during this dynamic melting and solidification process has been studied numerically in order to identify the dominating process parameters. Simulation tools based on a finite‐volume method have been developed to describe the heat transfer, fluid flow and the phase change during the melting and solidification of the ceramic. The results of the calculation have been validated against experimental results.     

铝合金焊前激光清洗的等离子体光谱在线检测

铝合金焊接技术在工业生产、制造和维修等领域有广泛的应用,焊缝内存在气孔导致焊接质量降低是铝合金焊接技术的常见问题。由于铝合金表面金属氧化物是导致气孔生成的主要来源,对激光清洗过程进行在线检测,不但可以实时分析表面氧化物的清洗状态,而且可以避免基体表面因为过度清洗造成损伤或二次氧化。提出采用激光诱导等离子体光谱(LIBS)在线检测铝合金焊前激光清洗过程,表征清洗后铝合金基体的表面状态。LIBS技术可以对多元素成分同时检测,拥有较低的检出限和较高的准确性。搭建基于Andor Mechelle 5000光谱仪的铝合金焊前激光清洗在线检测系统,剔除空气环境对实验结果的影响,测试6061铝合金表面氧化物和铝合金基体的LIBS光谱,分析两者独特的元素特征谱线,采用X射线能谱(EDS)测试结果验证元素特征谱线的准确性,并探讨激光清洗过程LIBS技术在线检测的可行性。实验测试等离子体光谱谱线强度与激光能量密度之间的关系,获得单次脉冲激光去除铝合金表面氧化物的损伤阈值,结合X射线能谱的检测结果研究激光损伤阈值的成因及影响。研究激光清洗过程等离子体光谱特征谱线与脉冲次数之间的关系,提出基于O/Al特征谱线强度比值作为在线检测清洗效果及二次氧化损伤的评判依据。为验证该评判依据的准确性,将O/Al特征谱线强度比值随清洗次数的变化趋势与X射线能谱测试获得的氧元素原子百分比变化趋势进行对比。实验结果表明:采用200~700 nm范围内激光诱导等离子体谱线特征分析激光清洗状态,可以剔除空气环境的影响;氧元素和铝元素特征谱线准确反映出表面氧化膜与铝合金基体的成分差异;X射线能谱检测元素成分和含量表明氧元素含量随着激光清洗能量密度先减后增,单次清洗铝合金的二次氧化损伤的激光能量阈值为11.46 J·cm-2,小于损伤阈值的激光能量密度对铝合金基体的多次清洗未造成损伤,等离子体光谱特征谱线强度与表面清洗状态相关, 656.5 nm(OⅡ)/396.2 nm(AlⅠ)谱线强度比值≤1.5%为激光清洗干净的依据。研究结果有利于铝合金的激光清洗实时控制技术和焊接装置集成化。     

Wide band gap and p‐type conductive Cu–Nb–O films

Cu–Nb–O films with a thickness of ca. 150 nm were prepared on borosilicate glass substrates using CuNbO₃ ceramic target at substrate temperature of 500 °C by pulsed laser deposition. The X‐ray diffraction patterns showed that the Cu–Nb–O films were amorphous or an aggregation of fine crystals. The post‐annealed film at 300 °C in N₂ gas showed 80% transmission in visible light (band gap = 2.6 eV) and high p‐type conductivity of 21 S cm^–1. The Cu–Nb–O film with a thickness of 100 nm, fabricated from the target with a composition of Cu/Nb = 0.9, showed the highest p‐type conductivity of 116 S cm^–1. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Fixation of bioactive calcium alkali phosphate on Ti6Al4V implant material with femtosecond laser pulses

Bone implants made of metal, often titanium or the titanium alloy Ti6Al4V, need to be surface treated to become bioactive. This enables the formation of a firm and durable connection of the prosthesis with the living bone. We present a new method to uniformly cover Ti6Al4V with a thin layer of ceramics that imitates bone material. These calcium alkali phosphates, called GB14 and Ca10, are applied to the metal by dip coating of metal plates into an aqueous slurry containing the fine ceramic powder. The dried samples are illuminated with the 790 nm radiation of a pulsed femtosecond laser. If the laser fluence is set to a value just below the ablation threshold of the ceramic (ca. 0.4 J/cm²) the 30 fs laser pulses penetrate the partly transparent ceramic layer of 20-40 μm thickness. The remaining laser fluence at the ceramic-metal interface is still high enough to generate a thin metal melt layer leading to the ceramic fixation on the metal. The laser processing step is only possible because Ti6Al4V has a lower ablation threshold (between 0.1 and 0.15 J/cm²) than the ceramic material. After laser treatment in a fluence range between 0.1 and 0.4 J/cm², only the particles in contact with the metal withstand a post-laser treatment (ultrasonic cleaning). The non-irradiated rest of the layer is washed off. In this work, we present results of a successful ceramic fixation extending over larger areas. This is fundamental for future applications of arbitrarily shaped implants.     

化学气相沉积SiC材料超光滑表面纳米加工

 利用传统光学加工方法，采用陶瓷磨盘和金刚石微粉对国产化学气相沉积(CVD) SiC进行了粗磨、细磨加工；然后，利用颗粒直径从4 μm到1 μm的金刚石研磨膏逐级进行抛光，发现SiC表面存在纳米级划痕；最后，改用颗粒直径为20 nm氧化铝纳米颗粒的碱性水溶液进行抛光，表面粗糙度达到0.6 nm(RMS)，表面纳米级划痕得到很好改善，获得了较高表面质量的超光滑表面。     

A Barrier Discharge Reactor with Ferroelectric Electrodes I. Influence of thickness and surface area of electrodes

A study aimed at finding a way of scaling-up a small laboratory reactor employing an electric discharge with a dielectric barrier was carried out. The dielectric used was ferroelectric ceramic material of a high permittivity (? above 1000) comparing to glass (? ≈? 3–10), which is generally used. The main component of the ceramics was BaTiO₃. The advantage of using this type of ceramics is related to a considerable increase in power density without the need of increasing voltage which supplies the system. The influence of the thickness and surface of ferroelectric electrodes on the macroscopic characteristics of the discharge and efficiency of chemical process was investigated. Ozone synthesis from oxygen was the reaction under consideration. A new structure of the reactor was proposed comprising a series of parallelly spaced thin ceramic plates. High electric permittivity of the ferroelectric ceramics enables such ?sandwich”? structure to be supplied by only two edge ceramic electrodes.     

Ti与莫来石陶瓷衬底的界面反应

在抛光的200℃莫来石陶瓷衬底上电子束蒸发淀积200nm的Ti膜，并在高真空中退火，利用二次离子质谱（SIMS）、俄歇电子能谱（AES）和X射线衍射分析（XRD）研究了从200—650℃Ti与莫来石的固相界面反应．结果表明，在淀积过程中，最初淀积的Ti与衬底表面的氧形成Ti—O键，并有微量元素态Al，Si原子析出，界面区很窄；450℃，1h退火后，界面区有所展宽，但变化不大；650℃，1h退火后，界面发生强烈反应，样品主要由TiO＋Ti，Ti₃Al，Ti₃Al＋TiSi₂和莫来石陶瓷衬底四层结构组成 关键词：     

激光诱导击穿光谱诊断合金铸件表面/界面质量

熔模精密铸造技术广泛应用于高温合金叶片生产。高温合金单晶叶片铸件尺寸精度高,内部和表面不得有缺陷,但在浇铸时易受浇铸温度场、熔体流场及与模壳发生界面反应的影响而导致表面结瘤、凹陷、缩孔等缺陷。激光诱导击穿光谱（LIBS）是一种非常有效的表面及界面分析技术,对于诊断分析铸件表面/界面质量具有明显的优势,对样品损伤小,可对不平整表面进行分析。研究优化了LIBS深度分析的条件,采用2 mm孔径光阑分光,500 mJ,1 064 nm脉冲高斯激光在焦外激发单晶高温合金获得了良好的空间分辨力,降低了能量密度较低的二级以上衍射环能量辐射造成表层烧蚀引起的深度分析信号失真。体积烧蚀速率与激光输出能量线性正相关,与光阑直径正相关,与激发频率无关。采用LIBS技术对DD407高温合金单晶叶片表面和近表面进行了深度分析。发现SiO₂-Al₂O₃莫来石结构的型壳在铸造过程中会引起DD407单晶叶片表面和近表面的Al,Ti,Ni,Cr,Co贫化,其中Al和Ti贫化显著且深度达50 μm。铸件尖锐部位较厚大部位的合金元素贫化明显。叶片经过脱芯脱壳后表面沉积钙镁盐类、钠盐物质。通过沸水清洗和超声清洗后,钠盐完全去除,钙镁物质均大幅减少,仍有3~5 μm厚。LIBS可方便的进行合金铸件表面和界面的成分分布分析,给出表面/界面质量的清晰判据,展现了较好的应用前景。     

Study of carrier concentration profiles in Al‐implanted Ge by micro‐Raman spectroscopy under different excitation wavelengths

The distribution profile of Al implanted in crystalline Ge has been investigated by micro‐Raman spectroscopy. Using different excitation laser lines, corresponding to different optical penetration depths, the Al concentration at different depths beneath the sample surface has been studied. We have found a strong correlation between the intensity of the Al–Ge Raman peak at ~370 cm⁻¹, which is due to the local vibrational mode of substitutional Al atoms, and the carrier concentration profile, obtained by the spreading resistance profiling analysis. A similar connection has been also observed for both shape and position of the Ge–Ge Raman peak at ~300 cm⁻¹. According to these experimental findings, we propose here a fast and nondestructive method, based on micro‐Raman spectroscopy under different excitation wavelengths, to estimate the carrier concentration profiles in Al‐implanted Ge. Copyright © 2013 John Wiley & Sons, Ltd.     

Characterization of laser processing of single‐crystal natural diamonds using micro‐Raman spectroscopic investigations

The application of lasers for processing diamond has revolutionized the diamond industry and its applications in microelectronics, microelectromechanical system (MEMS) and microoptoelectromechanical system (MOEMS) technologies. The process quality can be evaluated using spectroscopic techniques. In the present investigation, four different types of Q‐switched solid‐state lasers (with different beam parameters), namely, a lamp‐pumped Nd:YAG laser operating at 1064 nm, a lamp‐pumped Nd:YAG laser operating at second harmonically generated 532 nm, a diode‐pumped Nd:YVO₄ laser operating at 1064 nm and a diode‐pumped Nd:YAG laser operating at 1064 nm, have been employed for the processing of a single‐crystal, gem‐quality, natural diamond. The main objective behind the selection of these lasers with different beam parameters was to study the effect of wavelength, pulse width, pulse energy, peak power and beam quality factor (M² factor) on various aspects of processing (such as microcracking, material loss and cut surface quality) and their relative merits and demerits. The overall weight loss of the diamond and formation of microcracks during processing have been studied for the above four cases. The characteristics of the graphite formed during processing, elemental analysis, surface morphology of the cut surface and process dynamics have been studied using micro‐Raman spectroscopy and scanning electron microscopy (SEM). We observed that laser cutting of single‐crystal diamonds used for industrial applications can be accomplished without microcracking or surface distortion using Q‐switched Nd:YAG lasers. This allows direct processing without extensive postgrinding and polishing stages. Very efficient diamond processing is possible using diode‐pumped lasers, which results in the lowest possible breakage rate, good accuracy, good surface finish and low weight loss. From the micro‐Raman and SEM studies, it is concluded that the surface quality obtained is superior when diode‐pumped Nd:YVO₄ laser is used, owing to its extremely high peak power. The maximum graphite content is observed while processing with lamp‐pumped Nd:YAG laser at 532 nm. An overall comparison of all the laser sources leads to the conclusion that diode‐pumped Nd:YAG laser is a superior option for the efficient processing of natural diamond crystals. Copyright © 2006 John Wiley & Sons, Ltd.     

Laser processing of bulk Al–12Si alloy: influence of microstructure on thermal properties

The feasibility of enhancing the thermal conductivity of an alloy via microstructural refinement was examined using Al–12%Si alloy as a model material. Al–12Si alloy samples were fabricated at different process parameters using laser engineered net shaping (LENS?) and the effect of microstructural features on the thermal conductivity was studied and compared with conventionally cast alloy. The large difference in melting points and laser light absorptivities of Si and Al as well as the low melt viscosity of Al–12Si alloy resulted in a very small process window to successfully fabricate bulk Al–12Si alloy samples using LENS?. Comparison of microstructural features of laser-processed samples with cast Al–12Si alloy showed significant refinement in eutectic Si for laser processed samples. Microstructural refinement not only improved the thermal conductivity of Al–12Si alloy but also compensated the detrimental effect of porosity on thermal conductivity. The thermal conductivity of cast alloy varied between 82 and 93?W/mK, which is ～21–76% lower than the values exhibited by laser-processed samples in the range 103–153?W/mK. The results of LENS? fabrication, microstructural evolution and thermal properties of Al–12Si alloy bulk structures can be extended to other immiscible alloys and metal matrix composites for a variety of engineering applications.     

Surface cleaning and preparation in AlGaN/GaN-based HEMT processing as assessed by X-ray photoelectron spectroscopy

The chemical composition of the AlGaN/GaN surface during typical process steps in transistor fabrication was studied using X-ray photoelectron spectroscopy (XPS). The steps studied included organic solvent cleaning, 1:1 HCl:H₂O dip, buffered oxide etch dip, oxygen plasma descum and rapid thermal annealing (RTA). The surface composition was calculated after correction for the interference of the Ga Auger lines in the N 1s portion of the spectra. The buffered oxide etched (BOE) surface showed a greater tendency for Al (compared to Ga) to be oxidized in the surface, under a layer of adventitious carbon. Three different treatments were found to yield a combination of low C and O levels in the surface. Both plasma cleaning and RTA were highly effective at reducing the carbon contamination of the surface, but did increase the oxygen levels. The RTA treated surface was found to have low levels of oxygen incorporation to a depth of 2-6 nm.     

In situ XPS investigation of Pt(Sn)/Mg(Al)O catalysts during ethane dehydrogenation experiments

Calcined hydrotalcite with or without added metal (Mg(Al)O, Pt/Mg(Al)O and Pt,Sn/Mg(Al)O) have been investigated with in situ X-ray photoelectron spectroscopy (XPS) during ethane dehydrogenation experiments. The temperature in the analysis chamber was 450 °C and the gas pressure was in the range 0.3-1 mbar. Depth profiling of calcined hydrotalcite and platinum catalysts under reaction, oxidation and in hydrogen-water mixture was performed by varying the photon energy, covering an analysis depth of 10-21 Å. It was observed that the Mg/Al ratio in the Mg(Al)O crystallites does not vary significantly in the analysis depth range studied. This result indicates that Mg and Al are homogeneously distributed in the Mg(Al)O crystallites. Catalytic tests have shown that the initial activity of a Pt,Sn/Mg(Al)O catalyst increases during an activation period consisting of several cycles of reduction-dehydrogenation-oxidation. The Sn/Mg ratio in a Pt,Sn/Mg(Al)O catalyst was followed during several such cycles, and was found to increase during the activation period, probably due to a process where tin spreads over the carrier material and covers an increasing fraction of the Mg(Al)O surface. The results further indicate that spreading of tin occurs under reduction conditions.A PtSn₂ alloy was studied separately. The surface of the alloy was enriched in Sn during reduction and reaction conditions at 450 °C. Binding energies were determined and indicated that Sn on the particle surface is predominantly in an oxidised state under reaction conditions, while Pt and a fraction of Sn is present as a reduced Pt-Sn alloy.     

Free electron laser nitriding of metals: From basis physics to industrial applications

Titanium was laser nitrided by means of free-electron laser irradiation in pure nitrogen atmosphere. The variation of pulse frequency and macropulse duration of the free electron laser resulted in δ-TiN_x coatings with different thickness and different micro- and macroscopic morphologies. The coatings revealed, characteristic values for hardness, roughness and crystallographic texture, which originate from the growth mechanism, the solid-liquid interface energy and the strain. Further investigations showed that the dendritic growth is beginning at the surface and that the alignment of dendrites is normal to the surface. A correlation of the texture with the time structure of the laser pulses was found. Numerical simulations were performed and compared with the experimental results. The simulations can explain the experimental results.     

Light‐induced degradation and regeneration of multicrystalline silicon Al‐BSF and PERC solar cells

Light‐induced degradation (LID) is a well‐known problem faced by p‐type Czochralski (Cz) monocrystalline silicon (mono‐Si) wafer solar cells. In mono‐Si material, the physical mechanism has been traced to the formation of recombination active boron‐oxygen (B–O) complexes, which can be permanently deactivated through a regeneration process. In recent years, LID has also been identified to be a significant problem for multicrystalline silicon (multi‐Si) wafer solar cells, but the exact physical mechanism is still unknown. In this work, we study the effect of LID in two different solar cell structures, aluminium back‐surface‐field (Al‐BSF) and aluminium local back‐surface‐field (Al‐LBSF or PERC (passivated emitter and rear cell)) multi‐Si solar cells. The large‐area (156 mm × 156 mm) multi‐Si solar cells are light soaked under constant 1‐sun illumination at elevated temperatures of 90 °C. Our study shows that, in general, PERC multi‐Si solar cells degrade faster and to a greater extent than Al‐BSF multi‐Si solar cells. The total degradation and regeneration can occur within ～320 hours for PERC cells and within ～200 hours for Al‐BSF cells, which is much faster than the timescales previously reported for PERC cells. An important finding of this work is that Al‐BSF solar cells can also achieve almost complete regeneration, which has not been reported before. The maximum degradation in Al‐BSF cells is shown to reduce from 2% (relative) to an average of 1.5% (relative) with heavier phosphorus diffusion.     

Soft picosecond X-ray laser nanomodification of gold and aluminum surfaces

Experimental and theoretical investigations of aluminum (Al) and gold (Au) surface modification by soft X-ray laser pulse are presented. Well-polished samples of Al and Au are irradiated by ps-duration pulse with wavelength of 13.9 nm at the energy range of 24–72 nJ. Differences in the melting and the ablation processes for those materials are observed. It is shown that at low laser pulse energy, the nanoscale ripples on the surface may be induced by melting without following ablation. In that case, the nanoscale changes in the surface are caused by splash of molten metal under gradient of fluence. At higher laser pulse energy, the ablation process occurs and craters are formed on the surface. However, the melting determines the size of the modified surface at all ranges of the laser energies. For interpretation of experimental results, the atomistic simulations of melting and ablation processes in Al and Au are provided. The calculated threshold fluencies for melting and ablation are well consistent with measured ones.     

Impact of interfaces on nuclear materials

The vapor pressures and work function changes of the ceramic breeder materials, such as Li₄SiO₄, Li₂ZrO₃, Li₂TiO₃ and Li₂O at elevated temperatures were measured to investigate their thermochemical behavior. The experimentally obtained results of vapor pressures and work function changes were closely related to each other in terms of surface non-stoichiometry, indicating some relevance between macroscopic and microscopic behaviors of hydrogen at the surface of ceramic breeders.