不同气体环境下532nm激光诱导硅表面形貌的研究

研究了在不同气体环境下,利用532 nm Nd∶YAG纳秒脉冲激光累积辐照单晶硅表面形成的微结构,结果表明,在其他条件相同,背景气体不同的情况下,背景气体对硅表面形貌的形成起着重要的作用。具体分析了真空、N2和SF6 3种环境气氛下形成的微结构,结果显示,在SF6中形成的锥形微结构的数密度比在N2和真空中的大,并且锥形具有更大的纵横比;在N2、真空和SF6中形成的微结构尺寸依次减小。SF6气氛下,激光辅助化学刻蚀的效率比在真空和N2气氛中的高。另外,辐照区域边缘有波纹微结构形成,分析认为,该微结构的形成是由表面张力波的冷却导致的。     

不同气氛下飞秒激光诱导硅表面微结构

利用钛宝石飞秒激光脉冲对单晶硅在SF6、空气和真空环境中进行了累积脉冲辐照,研究了硅表面微结构的演化。在SF6气氛中,在激光辐照的初始阶段,硅表面形成了1维的波纹结构,随着辐照脉冲数的增加,波纹结构演化成了2维凹凸结构。累积600个脉冲后,硅表面产生了准规则排列且具有大纵横比的锥形尖峰结构。该结构呈现高度相对较低、锥形尖端小球不明显的特征,分析认为主要与环境气压的大小有关。对比空气、SF6和真空中的微结构发现,尖峰的数密度依次减小;SF6中形成的尖峰高度最大,其次为真空,再次为空气。研究结果表明,真空、SF6和空气3种环境下微结构的形成及表面形貌主要由激光烧蚀、化学刻蚀和氧化决定。     

纳秒激光脉冲诱导硅表面微结构

利用Nd:YAG纳秒激光脉冲,在能量密度为1～10 J/cm2范围内辐照单晶硅,形成了表面锥形微结构,在SF6气氛和空气环境下均形成了锥形尖峰表面微结构。SF6气氛下产生的锥形尖峰顶端都有小球,部分锥形上还有二次尖峰形成,空气中纳秒激光诱导的锥形尖峰微结构顶端和边缘有由液滴固化形成的粒状物质,不同于利用准分子纳秒激光诱导的细长须状结构和飞秒激光辐照下产生的具有表面枝蔓状纳米结构的锥形微结构。实验结果表明,这种尖峰微结构的形成与辐照激光的波长和脉冲持续时间有关。对空气中微构造硅的辐射反射的初步研究表明,在500～2 400 nm范围内的光辐射反射率不高于20%。     

Nd:YAG纳秒激光诱导硅表面微结构的演化

利用Nd:YAG纳秒激光(波长为532和355 nm)对单晶硅在真空中进行了累积脉冲辐照,研究了表面微结构的演化情况.在激光辐照的初始阶段,532和355 nm激光脉冲均在硅表面诱导出了波纹结构,后者辐照硅表面后形成了近似同心但稍显混乱的环形波纹结构.随着脉冲数的增加,波纹结构逐渐演化为一种类似珠形的凹凸结构,最后形成准规则排列的微米量级锥形结构,该微结构的生长依赖于表面张力波和结构自组织.分析发现,形成的交叉环形结构主要是在355 nm激光辐照硅的过程中,表面张力波导致波纹结构部分叠加的结果.     

1064 nm纳秒脉冲激光诱导硅表面微结构研究

利用Nd:YAG纳秒激光(波长为1064 nm)在不同气氛(空气、N₂,真空)中对单晶硅进行累积脉冲辐照,研究了表面微结构的演化情况.在激光辐照的初始阶段,与532和355 nm纳秒脉冲激光在硅表面诱导出波纹结构不同,1064 nm脉冲激光诱导出了微孔结构和折断线结构,并且硅的晶面取向不同,相应的折断线结构也不同.对于Si(111)面,两条折线交角为120°或60°,形成网状;而对于Si(100)面,两条折断线正交,从而将表面分成了15—20 μm的矩形块.结果表明,微孔结构的生长过程主要与相爆炸有关,而折断线的形成主要是热应力作用的结果.不同气氛对微结构形成的影响表明,刻蚀率和生长率与微结构的形成有密切的关系. 关键词： 纳秒激光 硅的微结构 相爆炸 热应力     

脉冲激光辐照硅材料引起表面波纹的特性研究

叙述了激光与材料相互作用过程中引起相干受激光散射的机制,以及形成材料表面波纹的特性。在激光波长1．06μm、能量15mJ、光斑直径2mm、脉冲半峰全宽约10ns和入射方向为布儒斯特角的条件下,进行了脉冲激光辐照硅材料形成表面波纹的实验研究。在脉冲激光辐照硅材料表面功率密度略大于材料损伤阈值的条件下,发现了硅材料表面形成的平行等间距直线条纹结构。用光学显微镜和原子力显微镜分别测量了被辐照硅材料表面的波纹形貌特征。在假设硅材料表面波纹的产生与声波在材料中的传播速度有关的条件下,由声波传播速度和激光辐照硅材料的脉冲宽度较好地解释了材料表面形成条纹的宽度．并认为在形成表面波纹的过程中,热应力起主要作用。     

单脉冲纳秒激光诱导硅表面微结构

利用Nd:YAG纳秒脉冲激光(波长532nm)在空气中对单晶硅表面进行单脉冲辐照,研究了激光能量密度和光斑面积变化对微结构的影响。通过场发射扫描电子显微镜和原子力显微镜(AFM)对样品表征,并对纳秒激光辐照硅的热力学过程进行分析。结果显示:当脉冲激光的能量密度接近硅的熔融阈值且光斑直径小于8μm时,形成尖峰微结构;随着能量密度或光斑面积增大,尖峰结构消失,形成边缘隆起和弹坑微结构。通过流体动力学模型得到微结构形貌的解析解,模拟得到的微结构形貌与实验测得的AFM数据一致。研究表明微结构的形成主要是由于表面张力引起的熔融硅流动。表面张力与表面温度和表面活性剂的质量浓度有关。温度梯度引起的热毛细流作用和表面活性剂浓度引起的毛细作用共同影响下形成尖峰、边缘隆起和弹坑微结构。     

532 nm纳秒激光辐照下的单晶硅表面微结构及荧光特性

采用Nd:YAG纳秒脉冲激光对单晶硅在空气中进行辐照,研究了表面微结构在不同能量密度和扫描速度下的演化情况。扫描电子显微镜测量表明,激光在相对较低能量密度下辐照硅表面诱导出鱼鳞状波纹结构,激光能量密度相对较大时,诱导出絮状多孔的不规则微结构。光致荧光谱（PL）表明,激光扫描区域在710 nm附近有荧光发射。用氢氟酸腐蚀掉样品表面的SiOx后,荧光峰的强度显著降低,说明SiOx在光致发光增强上起重要作用。能量色散X射线谱（EDS）表明氧元素的含量随激光能量密度的增大而增加。研究表明:纳秒激光的能量密度和扫描速度对微结构形成起着决定性作用,改变了硅材料表面微结构尺寸,增大了光吸收面积; 氧元素在光致发光增强上起重要作用,微构造硅和SiOx对光致荧光的发射都有贡献。     

飞秒脉冲激光辐照对硅发光性能的影响

利用飞秒脉冲激光对单晶硅进行辐照,研究了在不同环境(纯水和空气)和能量密度条件下激光刻蚀过后硅片的光致荧光特性.对于辐照后的硅片,利用了场发射扫描电子显微镜(FESEM)、能谱仪(EDS)、傅里叶红外光谱仪(FT-IR)、光致荧光光谱仪(PL)进行表征.结果显示:在空气中样品表面形成了条纹状微结构,纯水中硅片表面生成了尺寸更小的珊瑚状微结构;激光刻蚀后在硅片表面的生成物主要是SiOx(x2),在纯水中处理后硅片氧元素的含量接近是空气中的4倍;傅里叶变换红外透射谱中主要为Si—Si键(610 cm-1)和Si—O—Si键(1105 cm-1)的振动;在空气和纯水中激发出的荧光均为蓝光(420—470 nm),在各自最佳激发波长下,纯水中荧光强度比空气中强2到3倍,但是在可见光范围内荧光峰的位置和形状都基本没有发生变化.研究表明:氧元素在光致发光增强上起着重要作用,光致发光最主要是由形成的氧缺陷SiOx(x2)导致的,生成低值氧化物SiOx的多少决定了发光的强弱.     

飞秒激光作用下的硅表面微结构及发光特性

 采用近红外飞秒激光辐照浸泡在硫酸溶液中的N型单晶硅片，激光波长800 nm，脉宽200 fs，重频1 kHz，平均功率为100 mW,而硫酸溶液的质量分数分别选择为0.1%和1%。辐照后硅表面呈直径为5~8 mm,高度15 mm的柱型结构。分析其荧光特性，并通过比较硅材料表面微结构与激光光源、扫描参数、硅片背景环境的关系，确定最佳辐照条件为激光扫描速度750 mm/s,扫描间距5 mm/s。最终在厚度0.5 mm、直径26 mm的硅片上获得10 mm×10 mm的方形扫描区域，荧光光谱显示激光扫描后的区域在700 nm附近有很强的荧光发射。分析结果表明飞秒激光扫描改变了样品的表面微结构尺寸，增大了吸收面积，扩展了荧光激发波长，有效提高了样品的吸收效率和荧光发光相对强度(超过扫描前发光相对强度的2倍)，荧光发射谱的变化是由量子限制效应和表面态模型共同作用的结果。     

Transmission electron microscopy investigation of crystalline silicon surface irradiated by femtosecond laser pulses in different background atmospheres

This article aims to obtain structural and compositional characteristics of a crystalline silicon surface irradiated by femtosecond laser pulses in SF₆, N₂, air, and vacuum background atmospheres by performing transmission electron microscopy observation of ??110?? cross-sectional specimens. Conical microstructures covered with defective outer layers were formed in SF₆ gas. The elemental sulfur dopants in the surface microstructure, which located in close proximity to defects, were mainly concentrated at the tip region of the microcones, and about several hundred nanometers thick. In N₂ atmosphere, the defects produced regularly on the silicon surface were of the same types with those formed in SF₆ gas and confirmed to be stacking faults and overlapped twins. Furthermore, silicon crystalline grains with different orientations were observed on the silicon surface irradiated in N₂, air, and vacuum atmospheres. Especially, ??-Si₃N₄ crystalline grains were found to be formed in N₂ and air as chemical products when elemental nitrogen exists, and the SiO₂ amorphous phase was formed in air by the oxidation effect. Based on these experimental results, the relevant interaction mechanisms between pulsed laser and crystalline silicon were suggested to be mainly attributed to laser-assisted chemical etching and laser ablation, i.e., if volatile silicon compounds can be produced in a reactive gas atmosphere (e.g., SF₆), the strong laser-assisted chemical etching dominates over the laser irradiation process. Otherwise, laser ablation is the dominant mechanism such as in N₂, air, and vacuum.     

表面微构造的硅材料--一种新型的光电功能材料

在SF6气体氛围内用飞秒激光照射硅表面,可在硅表面产生准规则排列的微米量级尖峰结构,形成“黑硅”新材料．初步研究表明,这种“黑硅”新材料对波长为250-2500nm的光波有大于90％的吸收,同时它还具有相当好的场致发射特性．由于具有这些奇特的光电性质,这种表面微构造的硅材料在光电探测器、太阳能电池、平板显示器等器件制造领域有着重要的潜在应用价值．     

Effect of polarization on femtosecond laser pulses structuring silicon surface

Arrays of conical-like spikes can be formed on silicon surface after irradiated with femtosecond laser pulses in ambient of SF₆ or N₂. In this article, we report our observations on how the shape of the spikes formed on silicon surface varies with the polarization of laser beam. The experimental results show that, with circular polarized laser irradiation, the shape of the spikes is conical; however, with linearly polarized laser irradiation, the spikes show elliptic conical shape, and the long-axes are perpendicular to the direction of the polarization of laser beam. The asymmetric shape of spikes produced by linearly polarized laser beam can be explained by considering the polarization dependence of Fresnel-refraction.     

Formation of colorized silicon by femtosecond laser pulses in?different background gases

A single-crystal silicon(111) wafer surface fixed on an x–y translation stage is scanned with a focused femtosecond laser beam at a wavelength of 800 nm under different atmospheres (air, vacuum, and nitrogen). Different colors from different angles on the surface of the silicon then appear. From the result of the experiments, periodic ripple surface structures emerge on the surface of colorized silicon, and the phenomenon is more obvious in vacuum and nitrogen than in air. The periods of the surface structures on silicon are not the same in the different atmospheres. Under vacuum, the period is the longest and is closer to the wavelength of the laser irradiation. Different from metals, the range of energy density is smaller when the colorized silicon appears with femtosecond laser pulses. Through SEM, TEM, and AFM, we observe in detail the microstructures of colorized silicon that forms in air, vacuum, and nitrogen and analyze the possible physical mechanism. Finally, research into the optical reflection of the colorized silicon indicates that the reflectivity is not higher than 30% in the 250–800 nm range.     

Formation of nano-textured conical microstructures in titanium metal surface by femtosecond laser irradiation

We report for the first time that a regular array of sharp nano-textured conical microstructures are formed on the titanium metal surface by irradiation with ultrafast laser pulses of 130 fs duration, 800 nm wavelength in vacuum (∼1 mbar) or in 100 mbar He. The microstructures are up to 25 μm tall, and taper to about 500 nm diameters at the tip. Irradiation in the presence of SF₆, air or HCl creates a textured surface but does not create sharp conical microstructures. The surfaces of these microstructures exhibit periodic nano-texture of feature size comparable to the wavelength of light consistent with ripple formation. Contrary to pillar formation by femtosecond laser irradiation of silicon where the initial ripples evolve into the pillars and the ripples disappear, the ripples on titanium pillars have a much smaller periodicity than the pillars and remain on the surface of the pillars. The textured surface is pitch black compared to its original silver-grayish color, i.e, it exhibits greatly reduced reflectivity throughout the measured visible spectrum. PACS 52.38.Mf; 79.20.Ds; 81.07.-b; 81.16.-c; 82.53.-k     

Ultrahigh infrared normal spectral emissivity of microstructured silicon coating Au film

We studied infrared normal spectral emissivity on quasi-periodic microstructured silicon, which was prepared by femtosecond laser irradiation in SF6 ambient gas, coated with 100 nm thick Au thin film. The observed emissivity is higher than any reported previously for a flat material with a thickness of less than 0.5 mm, at a temperature range of 200 °C to 400 °C. The emissivity over the measured wavelength region increases with temperature and the spike height. These results show the potential to be used as a flat blackbody source or for applications in infrared thermal sensor, detector, and stealth military technology.