Optical characterization and laser damage of fused silica optics after ion beam sputtering

The sputtering process of fused silica bombarded by Ar ion beam is simulated with the SRIM software. The effects of ion beam energy and incident angle on sputtering yield and surface damage are computed. Since ion beam sputtering will result in defects in fused silica, such as E′ color centers and other lattice defects and probably Argon bubbles, the optimized sputtering energy is selected below 1 keV so that the projected range of Ar ions is less than 10 Å. The experimental results show that the scratches in subsurface of fused silica can be smoothed obviously and better surface can be obtained as the optimized parameters are used for ion beam sputtering. The laser induced damage threshold of fused silica increases by about 18% after ion beam sputtering.     

Superficial defects induced by argon and oxygen bombardments on (110) TiO2 surfaces

Compositional and chemical changes of titanium dioxide monocrystalline surfaces induced by bombardment with 4 keV argon and oxygen ions have been studied by AES, XPS and AFM. Argon ion bombardment induced strong changes in the composition and chemical state of the surface: loss of oxygen due to preferential sputtering occurred, and, related to this, Ti⁴⁺ species were reduced to Ti³⁺ and Ti²⁺. During oxygen bombardment, competition between preferential sputtering of oxygen ions of the oxide surface and oxygen implantation was observed. This phenomenon was found to be strongly dependent upon the incidence angle of the oxygen ions. Moreover, an oxygen bombardment with normal incidence of the surface that had been previously submitted to an argon ion bombardment led to a restoichiometrization of the surface: no further Ti³⁺ or Ti²⁺ was found by XPS, only Ti⁴⁺.     

Mechanism of defect evolution in H+ and He+ implanted InP

The defect evolution in InP with the 75 keV H⁺ and 115 keV He⁺ implantation at room temperature after subsequent annealing has been investigated in detail. With the same ion implantation fluence, the He⁺ implantation caused much broader damage distribution accompanied by much higher out-of-plane strain with respect to the H⁺ implanted InP. After annealing, the H⁺ implanted InP did not show any blistering or exfoliation on the surface even at the high fluence and the H₂ molecules were stored in the heterogeneously oriented platelet defects. However, the He molecules were stored into the large bubbles which relaxed toward the free surface, creating blisters at the high fluence.     

光学玻璃基底原子层同质材料沉积薄膜光谱及激光诱导损伤特性研究

通过原子层沉积技术在熔石英玻璃表面制备了同质材料的单层SiO₂薄膜,对光学薄膜的物理化学性质和强激光辐照下的激光诱导损伤性能进行了深入研究。实验中采用双叔丁基氨基硅烷（BTBAS）和臭氧（O₃）作为反应前驱体,在熔石英光学元件表面进行了SiO₂薄膜的原子层沉积工艺研究,以不同沉积温度条件制备了一系列膜样品。首先对原子层沉积特性和薄膜均匀性展开了研究,发现薄膜生长厚度与沉积循环次数之间符合线性生长规律,验证了制备薄膜的原子级逐层生长特性,并且表面沉积膜层的均匀性很好,其测得膜厚波动不超过2%。然后针对不同温度条件下沉积的SiO₂薄膜,对其粗糙度及各类光谱特性展开了研究,对比结果表明：样品的表面粗糙度在镀膜后有轻微的降低;薄膜样品在200～1 000 nm范围内具有出色的透过率,均超过90%并逐渐趋近于93.3%,且其透射光谱与在裸露熔石英衬底上测得的光谱没有明显差异;镀膜前后荧光光谱和傅里叶变换红外光谱的差异证实了原子层沉积SiO₂膜中点缺陷（非桥键氧、氧空位、羟基等）的存在,这将会影响薄膜耐损伤性能。最后对衬底和膜样品进行了紫外激光诱导损伤测试,损伤阈值的变化表明熔石英元件表面沉积薄膜后的激光损伤性能有所降低,其零概率损伤阈值从31.8 J·cm-2减小到20 J·cm-2左右,与光谱缺陷情况表征相符合。薄膜中点缺陷部位会吸收紫外激光能量,导致局域温度升高,进而出现激光诱导损伤现象并降低抗激光损伤阈值。在选定的沉积温度范围内,较高温度条件下沉积的SiO₂薄膜其激光诱导损伤性能更好,可以控制沉积温度条件使得元件的抗损伤性能更为接近衬底本身,后续有望通过其他反应参数的优化来获得薄膜抗损伤性能的进一步提升。     

Low sputter damage of metal single crystalline surfaces investigated with medium energy ion scattering spectroscopy

It was observed clearly that the sputter damage due to Ar⁺ ion bombardment on metal single crystalline surfaces is extremely low and the local surface atomic structure is preserved, which is totally different from semiconductor single crystalline surfaces. Medium energy ion scattering spectroscopy (MEIS) shows that there is little irradiation damage on the metal single crystalline surfaces such as Pt(111), Pt(100), and Cu(111), in contrast to the semiconductor Si(100) surfaces, for the ion energy of 3–7 keV even above 10¹⁶–10¹⁷ ions/cm² ion doses at room temperature. However, low energy electron diffraction (LEED) spots became blurred after bombardment. Transmission Electron Microscopy (TEM) studies of a Pt polycrystalline thin film showed formation of dislocations after sputtering. Complementary MEIS, LEED and TEM data show that on sputtered single-crystal metal surfaces, metal atoms recrystallize at room temperature after each ion impact. After repeated ion impacts, local defects accumulate to degrade long range orders.     

Creation of variable concentrations of defects on TiO2(110) using low-density electron beams

Low density (˜μA/cm²) 0.48 and 1.0 keV electron beams have been used to create surface defects on a TiO₂(110) surface. These electron-beam induced defects were examined primarily by X-ray photoelectron spectroscopy (XPS) with supporting ultraviolet photoemission spectroscopy (UPS). Glancing and normal emission XPS spectra of nearly defect-free surfaces revealed that Ti atoms on the surface were similar to the bulk Ti, while some surface oxygen atoms were different from the bulk oxygen. XPS of Ti 2p_3/2 was used to quantify the defect concentration and to examine the defect electronic structure. Based on our calculation of defect concentrations and the comparison of our results with results and models from the literature, we conclude that oxygen vacancies induced by electron beams in the current study are mostly from the bridging oxygen sites, in agreement with the previous work. A range of defect concentrations with similar electronic structure, mainly composed of Ti³⁺, have been induced by low-density electron beams. Beam energy and exposure were the experimental variables. The rates of defect formation at low beam exposure were beam-energy dependent, with a faster growth rate at 0.48 keV than at 1.0 keV. These defects were similar to those by thermal annealing in vacuum, but a higher concentration of defects could be obtained with longer beam exposure. However, the e-beam induced defects were different from those produced by Ar⁺ ion bombardment since both this and previous studies have found defects produced by Ar⁺ ion bombardment to be complex, with a variety of different local environments where oxygen and titanium surface atoms coexist.     

预应力对熔石英损伤的影响

采用ANSYS进行形变-应力模拟。对不同应力状态下的熔石英表面进行三倍频激光损伤测试,结果发现,预加压应力为0~50 MPa时损伤阈值有明显提高的趋势,用应力耦合作用对此给出了解释:0~50 MPa的预加压应力可以降低和抵消激光辐照产生的张应力破坏,大于50 MPa预应力的耦合作用会使得该处机械性能下降,另外,损伤增长在预应力存在时更容易发生。因此,0~50 MPa预加压应力时的表面预应力可以提高熔石英的抗激光辐照能力。     

The effect of nitrogen ion implantation on tungsten surfaces

X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were used to study the phase, composition and chemical states of elements at the tungsten surface. The measurement results indicate that nitrogen-containing phase of tungsten were formed by nitrogen ion implantation (energy 40 keV, implantation doses of 4×10¹⁷, 8×10¹⁷ and 1.6×10¹⁸ ions/cm²). The formation of the W_x(O,N) and WN in the surface layer occurred as a result of nitrogen ion irradiation. A decrease in concentration of W_x(O,N) is observed with increasing N⁺ while that WN increases. Due to residual oxygen in the chamber WO₃ still exists at the surface of the specimen.     

表面粗糙度对面向等离子体钨材料溅射的影响

依据钨材料表面溅射的实验现象,建立钨材料表面粗糙模型,模拟了高能H⁺、He⁺粒子辐照下的钨材料表面的溅射行为过程,并与基于离子输运的双群模型计算得到的结果作了比较。结果表明,随着钨材料表面粗糙程度的增加,溅射率降低;对一定的粗糙表面,相同能量的不同入射粒子,质量越大粒子溅射率越高,这些结果为分析聚变装置中心等离子体杂质水平和评价偏滤器寿命等提供了一定的理论支撑。     

熔石英表面铜膜污染物诱导损伤实验研究

 在熔石英元件表面溅射一层厚度小于10 nm的金属铜膜污染物,并测试元件的透过率。测试355 nm熔石英元件的激光损伤阈值,并用光学显微镜观测损伤形态。实验结果表明：污染后的熔石英元件的损伤阈值降低20%左右,元件表面的金属污染物薄膜经强激光辐照,在熔石英表面形成很多坑状微损伤,分布不均的热应力导致表面起伏,并有明显的烧蚀现象,导致基底损伤阈值下降。建立的光吸收和热沉积传输模型初步解释污染物膜层导致熔石英元件损伤的机理。     

Electrical characterization of argon-ion sputtered n-GaAs

Epitaxially grown n-type GaAs was sputtered with 0.5 keV Ar ions at doses of 10¹² and 10¹⁵ ions/cm². The sputter-induced defects in the GaAs were characterized using deep-level transient spectroscopy (DLTS) and the effect of these defects on the characteristics of Au Schottky barrier diodes (SBD's) fabricated on the sputtered GaAs was evaluated by current-voltage measurements. It was found that the barrier height of the SBD's decreased with ion dose from 0.97 eV for unsputtered diodes to 0.48 eV after sputtering at a dose of 10¹⁵/cm². DLTS showed the presence of a multitude of sputter-induced defects at and near the GaAs surface. The defects formed during the initial stages of sputtering had the same properties as some of the primary defects introduced during electron and proton irradiation of GaAs. Isochronal annealing at temperatures of up to 350°C showed that although some defects were removed by annealing, others appeared.     

Investigation of relative sputtering yields during ionoluminescence of Si

Atomic line emissions resulting from sputtered atoms and ions are investigated on Si(100) bombarded by 60 keV Ne⁺, 300 keV Xe⁺ and 300 keV SF₅⁺ ions. It has been observed that the presence of oxygen enhances light emission due to radiative de-excitation. Relative sputtering yields of Si for 60 keV Ne⁺, 300 keV Xe⁺ and 300 keV SF₅⁺ are estimated from the photon yields. The estimates of sputtering yields of adsorbed oxygen on Si for the above projectiles are also made from the transients of Si I 251.6 nm line. A non-linearity in the sputtering yield for SF₅⁺ ions was observed in comparison with the yields for Ne⁺ and Xe⁺ ions. The results are discussed with the model of overlapping of individual collision cascades.     

Surface defects created by low energy (20 < E < 240 eV) ion bombardment of Ge(001)

Surface defects created on Ge(001) exposed to low energy Xe ions are characterized by in situ scanning tunneling microscopy (STM). The temperature of the sample during ion bombardment is 165 C and ion energies range from 20 to 240 eV. The ion collisions create defects (vacancies and adatoms) which nucleate and form vacancy and adatom islands. For fixed total vacancy creation, the vacancy island number density increases with increasing ion energy: the vacancy island number density is 1.6 × 10⁻²⁰ cm⁻² for 40 eV ion bombardment and increases to 4.4 × 10⁻²⁰ cm⁻² for 240 eV ion bombardment. The increased nucleation rate for vacancies is attributed to clustering of defects. The sputtering yield of Ge(001) is also measured by STM. The sputtering yield for 20 eV ions is approximately 10⁻³ per ion but the net yield for surface defects (sum of adatoms and vacancies) is an order of magnitude higher, 10⁻², due to adatom-vacancy pair creation.     

表面Al膜污染物诱导熔石英表面损伤特性

在熔石英表面人工溅射一层Al膜污染物,分别测试污染前后熔石英基片在355 nm波长激光辐照下的损伤阈值,并采用透射式光热透镜技术、椭偏仪和光学显微镜研究了污染物Al膜的热吸收、厚度以及激光辐照前后熔石英的损伤形貌。用355 nm波长的脉冲激光分别辐照位于污染的熔石英和洁净的熔石英前后表面的损伤点,并用显微镜在线采集损伤增长图样,测试损伤点面积。实验表明:熔石英前表面的金属Al膜污染物导致基片损伤阈值的下降约30%,后表面的污染物导致基片下降约15%,位于熔石英样片后表面损伤点面积随激光辐照次数呈指数增长,而位于前表面的损伤点面积与激光脉冲辐照次数呈线性增长关系;带有污染的熔石英样片的增长因子比洁净的熔石英样片的增长因子高30%。     

1064 nm和532 nm纳秒激光同时辐照熔石英损伤规律的研究

利用Nd: YAG激光器研究基频(1064 nm)与倍频(532 nm)单独辐照和同时辐照下熔石英的损伤规律,对损伤几率进行了测试,获得损伤几率曲线与典型损伤形貌。研究结果表明:双波长同时辐照下的初始损伤阈值总是小于单波长辐照下的初始损伤阈值;基频光中加入定量倍频光后,熔石英对基频光的吸收效率提高;并且双波长同时辐照下,熔石英损伤密度增大;原因主要是熔石英表面缺陷对不同波长吸收机制的差异。     

Creating homogeneous depth profiles in YBaCuO films by ion beam implantation for uniform supression of Tc

Critical temperature depth profiles were calculated for single and multiple energy oxygen ion implantation of YBaCuO thin films. Using the code and the diffusion equation the changes of the profiles during an annealing between 150 and 300°C were obtained. The results are in reasonable agreement with the experimental data. Experimentally we investigated further implantation of O⁺, Ne⁺ and Al⁺ with a homogeneous implantation profile. The critical temperature is depressed by the created defects and in the case of Al also by substitution of Cu. For O⁺ and Ne⁺ implantation the depression of the critical temperature is diminished by an annealing process. Depending on the quality of the films, T_c reaches in some cases the values of the unimplanted samples. For Al⁺ the critical temperature changes less by the annealing process compared to the O⁺ or Ne⁺ implantations and does not reach the starting values. Some results of an annealing made by laser treatment are presented, too.     

Subsurface defect characterization and laser-induced damage performance of fused silica optics polished with colloidal silica and ceria

This paper mainly focuses on the influence of colloidal silica polishing on the damage performance of fused silica optics. In this paper, nanometer sized colloidal silica and micron sized ceria are used to polish fused silica optics. The colloidal silica polished samples and ceria polished samples exhibit that the root-mean-squared(RMS) average surface roughness values are 0.7 nm and 1.0 nm, respectively. The subsurface defects and damage performance of the polished optics are analyzed and discussed. It is revealed that colloidal silica polishing will introduce much fewer absorptive contaminant elements and subsurface damages especially no trailing indentation fracture. The 355-nm laser damage test reveals that each of the fused silica samples polished with colloidal silica has a much higher damage threshold and lower damage density than ceria polished samples. Colloidal silica polishing is potential in manufacturing high power laser optics.     

大口径氘化磷酸二氢钾晶体离线亚纳秒激光预处理技术

大口径氘化磷酸二氢钾(DKDP)晶体抗激光损伤性能偏低严重地制约着大型高功率激光装置输出水平.本研究利用离线亚纳秒激光预处理技术有效地提升了大口径DKDP晶体抗激光损伤性能.实际使用情况表明,采用离线亚纳秒激光预处理后,DKDP晶体在9 J/cm²激光通量辐照下的表面平均损伤密度得到大幅下降,由未处理前的5.02 pp/cm²(1pp表示1个百分点)降至0.55 pp/cm²,降幅为一个数量级.同时,激光预处理对晶体损伤尺寸具有一定的抑制作用,预处理后晶体损伤点尺寸分布曲线向尺寸减小的方向平移,尺寸分布峰值由预处理前的25μm降至预处理后的18—20μm.     

Dependence of Auger depth resolution and surface texturing on primary ion species

The dependence of Auger depth resolution and surface texturing on primary ion species was systematically investigated for polycrystalline Al, Mo, Ag and Ta films deposited on Si wafers, using 3 keV Ne⁺, Ar⁺ and Xe⁺ ions as projectiles. The resolution was found to depend strongly on ion species; the higher the ion mass, the better the resolution. The resolution improvement attained with Xe⁺ ions was dramatic for Al, becoming less pronounced for higher mass targets. As revealed by high-resolution scanning electron microscopy, Xe⁺ sputtering led to less-developed topographical structures of sputtered areas, which allowed us to conclude that ion sputtering with heavier ions roughens the surface less, resulting in a marked improvement in resolution.     

氦离子显微镜对钨中氦行为的实验研究

针对热核聚变面向等离子体钨材料中氦泡形成、演变以及机理研究的需求,克服目前常用离子注入、电子扫描显微镜和透射电子显微镜等离线研究手段存在的不足,提出氦离子显微镜对钨中氦的上述行为原位实时在线研究方法.借助氦离子显微镜的离子注入、显微成像和聚焦离子束纳米加工功能,它可以提供能量为0.5—35 ke V、束流密度可达10~(25) ions/(m~2·s)以上的氦离子束,在该设备上进行钨中氦的注入实验.同时在注入过程,实时在线监测钨中氦泡形成、演变过程以及钨材料表面形貌的变化,原位在线分析钨材料表面氦泡的大小、迁移合并以及其诱发的钨表面和近表面的微观损伤.实验结果表明:氦离子显微镜是研究钨中氦行为演变过程及其微观机理研究的新的研究手段和强有力的实验工具.