HF酸刻蚀提升熔石英亚表面划痕抗损伤性能的机理

用HF酸刻蚀熔石英元件,研究刻蚀对元件后表面划痕的形貌结构及损伤性能的影响,探索损伤阈值提升的原因.时域有限差分算法理论计算结果表明:对于含有50nm直径氧化锆颗粒的划痕,对入射光调制引发场增强的最大值是入射光强的6.1倍,且最强点位于划痕内部氧化锆颗粒附近,而结构相同但不含杂质的划痕引发的最大场增强为入射光强的3.6倍,最强区位于划痕外围;HF酸刻蚀能够有效去除划痕中的杂质,改变划痕结构,增加其宽深比值,经刻蚀的划痕对入射光调制引发场增强降低到入射光强的2.2倍.实验结果表明,经过深度刻蚀的划痕初始损伤阈值较刻蚀之前提高一倍多;光热弱吸收测试仪测试刻蚀后划痕对1 064nm激光的吸收最大值仅为230ppm.HF酸刻蚀同时可以提升元件整体损伤阈值,由于元件上无缺陷区域损伤阈值随刻蚀的深入先增加后降低,因此HF酸刻蚀应进行到元件损伤阈值提升到最大值为止.     

激光诱导HF酸刻蚀后熔石英后表面划痕的损伤行为研究

用光学显微镜和原子力显微镜记录HF酸刻蚀后熔石英元件后表面划痕的形貌结构,并利用单脉冲激光对其进行辐照测试,以研究不同结构参数划痕的激光损伤特性.实验结果表明,由于HF酸的腐蚀钝化作用,划痕结构横向截面呈余弦形分布;其初始损伤阈值并非由单一的划痕宽度或深度参数决定,而是与其横向剖面结构的宽深比值密切相关;通过实验得到了二者之间的关系曲线,并采用时域有限差分算法对不同结构参数划痕附近光场分布进行理论模拟,理论场计算得到的增强结果与实验值符合得很好.     

熔石英亚表面划痕激光诱导损伤阈值实验研究

用原子力显微镜和光学显微镜观测酸蚀后熔石英亚表面划痕,并根据形貌特征将其分为Boussinesq-point-force crack(BPFC)、Hertzian-conical scratch(HCS)和Plastic indent(PI)三类,测试了各类划痕的损伤阈值,讨论了激光损伤机制。结果表明锐度较大的BPFC损伤阈值不超过2.0 J/cm<>2;深度小于1 μm的 HCS阈值可达2.6 J/cm2;形变较大的PI阈值至2.8 J/cm2,形变较小的PI的激光损伤阈值与无缺陷材料相当。BPFC 和深度超过1 μm的HCS是导致熔石英损伤阈值低的主要因素。     

熔石英亚表面划痕激光诱导损伤阈值实验研究

 用原子力显微镜和光学显微镜观测酸蚀后熔石英亚表面划痕,并根据形貌特征将其分为Boussinesq-point-force crack(BPFC)、Hertzian-conical scratch(HCS)和Plastic indent(PI)三类,测试了各类划痕的损伤阈值,讨论了激光损伤机制。结果表明锐度较大的BPFC损伤阈值不超过2.0 J/cm<>2;深度小于1 μm的 HCS阈值可达2.6 J/cm²;形变较大的PI阈值至2.8 J/cm2,形变较小的PI的激光损伤阈值与无缺陷材料相当。BPFC 和深度超过1 μm的HCS是导致熔石英损伤阈值低的主要因素。     

熔石英元件HF刻蚀的实验研究

为深入了解熔石英元件化学刻蚀过程,研究了HF刻蚀反应机理、HF刻蚀工艺参数以及刻蚀对表面质量的影响规律。通过控制变量法,获得刻蚀速率随HF浓度、刻蚀温度以及NH4F浓度的变化规律。对刻蚀不同深度后的元件表面粗糙度、形貌、杂质含量以及激光损伤阈值进行了检测,实验结果表明：刻蚀速率受多种因素共同影响,其中HF浓度的促进作用最为显著;刻蚀后的熔石英表面形貌复杂,有横向、纵向、拖尾等形式的划痕,以及坑点、杂质等缺陷,其中横向划痕和纵向划痕占据了缺陷部分的主体,主要杂质铈元素随刻蚀时间的增长不断减少;激光损伤阈值测量实验表明,通过HF刻蚀将元件损伤阈值提高了59.6%。     

熔石英亚表面横向划痕调制作用的3维模拟

建立了熔石英后表面3维横向划痕模型,并采用3维时域有限差分方法对熔石英亚表面划痕周围的电场强度进行了数值模拟,分析了划痕宽度、深度、长度以及划痕倾斜角度对入射光场的调制作用,结果表明:随划痕深度和划痕长度的增加,熔石英内的最大电场强度增大,且当划痕长度达到1μm以上时,最大电场强度趋于稳定;划痕结构因子在1~2之间的划痕较容易引起熔石英损伤;而入射激光在划痕界面和后表面之间发生内全反射时,后表面上的光强增强效果更加明显,因此减少角度范围在20.9°~45°之内的划痕能大幅提高熔石英的损伤阈值。     

熔石英亚表面横向划痕调制作用的3维模拟

建立了熔石英后表面3维横向划痕模型,并采用3维时域有限差分方法对熔石英亚表面划痕周围的电场强度进行了数值模拟,分析了划痕宽度、深度、长度以及划痕倾斜角度对入射光场的调制作用,结果表明：随划痕深度和划痕长度的增加,熔石英内的最大电场强度增大,且当划痕长度达到1 μm以上时,最大电场强度趋于稳定;划痕结构因子在1～2之间的划痕较容易引起熔石英损伤;而入射激光在划痕界面和后表面之间发生内全反射时,后表面上的光强增强效果更加明显,因此减少角度范围在20.9°～45°之内的划痕能大幅提高熔石英的损伤阈值。     

静/动态刻蚀对熔石英表面质量和激光损伤的影响

为了研究静/动态刻蚀过程中熔石英表面质量和抗激光损伤性能的演变规律,优化化学刻蚀工艺,使用HF酸缓冲液对熔石英分别进行了不同时间的静/动态刻蚀处理。实验表明,由于兆声场辅助搅拌作用,熔石英动态刻蚀的刻蚀速率快于静态刻蚀。动态刻蚀后熔石英表面均方根(RMS)粗糙度和反射面形分别为 < 1 nm和0.46λ,其3倍频透射率先小幅增加后保持稳定,相比初始表面增加约0.1%。而静态刻蚀使得表面RMS粗糙度和反射面形分别增加至~5 nm和0.82λ,其3倍频透射率先基本不变后下降,相比初始表面下降约0.4%。二者损伤阈值呈现明显不同变化规律:静态刻蚀使熔石英损伤阈值先小幅增加约30%后逐渐降低,动态刻蚀使熔石英损伤阈值增加近一倍后保持相对稳定。结果表明,动态刻蚀后熔石英光学元件性能明显优于静态刻蚀。     

熔石英的快速激光刻蚀

使用10.6μm连续波CO_2激光和几种工作气体,对熔石英实现了快速的激光刻蚀.得到了刻蚀速度高于200μm/s的干净、光滑的表面;并根据所提出的机理对观察到的实验结果进行了解释.     

熔石英元件抛光表面的亚表面损伤研究

通过结合HF酸洗和微分干涉差显微成像对两组抛光元件的亚表面损伤进行直接观测和分析。结果显示微分干涉差显微成像相比于传统的明场成像具有更好的分辨率,可以更有效检测HF酸洗后暴露的各种浅塑性亚表面损伤。对两组抛光元件的亚表面损伤的对比分析发现熔石英元件在抛光中会产生大量的亚表面损伤,这些亚表面损伤绝大多数是浅塑性的划痕和坑,仅有少量的脆性断裂损伤,较大的抛光颗粒会产生更多更严重的亚表面损伤,并且这些亚表面损伤被表面沉积层所掩盖,表面粗糙度不能反映亚表面损伤的严重程度。     

Cu2+离子注入的石英光波导的特性研究

利用Cu2+离子注入的方式在熔融石英和石英晶体上分别制备了平面光波导结构.通过棱镜耦合实验测试了两种光波导的导模特性,结果表明:在同样的注入条件下熔融石英上形成了增加型的光波导结构,而石英晶体上形成了位垒型的光波导结构.研究了退火温度对两种光波导导模折射率的影响,熔融石英光波导中导模的折射率随着退火温度的升高而降低,而石英晶体光波导中导模的折射率随着退火温度的升高先增加后降低.为了进一步分析离子注入两种材料形成光波导的微观机理,利用SRIM模拟了Cu2+离子注入两种材料的电子能量损失和核能量损失,并且模拟了两种光波导结构的折射率分布.模拟结果表明:熔融石英光波导的主要形成原因是离子注入表面的折射率大于其体材料的折射率,而石英晶体光波导的主要形成原因是离子射程末端的折射率小于其体材料的折射率.因此,在熔融石英光波导的形成中电子能量损失起主要作用,而在石英晶体光波导的形成中核能量损失起主要作用.     

飞秒激光脉冲诱导透明介质的非线性吸收和折射率改变轮廓研究

实验研究了飞秒激光脉冲诱导熔融石英的非线性吸收特性,利用激光诱导自由电子等离子体浓度取决于多光子吸收系数和入射光强的关系;数值模拟了激光诱导折射率变化区域的大小,结合非线性吸收机理和飞秒激光脉冲与介质的相互作用,解释了飞秒激光脉冲超精细加工不受衍射极限的约束,可实现纳米级加工的机理结果表明,电介质的电离能越大,飞秒脉冲诱导的折射率变化区域就越小,但要求的激光脉冲能量也越大;为飞秒激光脉冲超精细加工的材料和激光参量选择提供了理论依据.     

三种不同波长的激光对熔石英损伤行为的对比研究

利用SAGA激光器,输出脉宽为7．2ns、波长分别为1064nm、532nm、355nm的基频光和倍频光,对相同类型的5块石英基片用R：1的方法分别测量了其损伤阂值,对比不同波长激光对石英材料的损伤行为差异。得出其损伤阈值在三种不同波长激光作用下分别为：46．78J／cm^2、13．4J／cm^2、9．28J／cm^2;并利用尼康E600W光学显微镜对三种不同波长激光造成的损伤形貌进行了观察,结合当前光学材料的损伤机理,对比得出倍频激光对石英基片的损伤破坏能力远大于基频光,且对石英材料的损伤机理主要表现为多光子吸收导致的雪崩电离破坏,而基频光的损伤多为表面缺陷及杂质引起的热破坏的结论。     

基频和三倍频Nd:YAG激光诱导熔石英损伤特性

 采用光电探测器和数字示波器检测散射光脉冲信号,研究了基频和三倍频Nd:YAG激光诱导熔石英损伤过程,给出了泵浦光和探针光的散射光光电信号;比较了基频和三倍频激光作用下熔石英烧蚀斑显微照片,并分析了其损伤机理。结果显示:在ns脉冲激光作用下,熔石英损伤均发生在泵浦激光脉冲峰值附近,且基频光作用下损伤开始时间点比三倍频作用下早;在多脉冲或高能量激光辐照下,检测到了等离子体闪光信号,等离子体闪光发生在时间延迟21 ns附近。基于Keldysh理论计算了基频光和三倍频光作用下,熔石英光致电离速率同激光强度的关系。     

熔石英光学材料紫外皮秒激光损伤的瞬态特性研究

光学元件激光损伤是限制高功率激光装置输出能力的关键因素,为了理解光学元件激光损伤过程,提高光学元件抗激光损伤性能,利用偏振阴影显微镜成像技术和光电探测技术研究了紫外皮秒激光诱使熔石英光学元件损伤的时间分辨动力学过程。结果显示了紫外皮秒激光作用过程中冲击应力波的传输特性、瞬态吸收的演变过程以及裂缝的发展过程。结果表明,冲击应力波的传输速度约为6.9μm/ns;532nm波长的激光瞬态吸收在激光作用之后2.5μs时激光吸收达到最大值,之后缓慢下降,整个持续时间可达50μs以上;损伤裂纹在7.5ns时刻就基本停止增长。研究结果对理解皮秒激光的损伤机制有重要意义。     

Preparation and Properties of Polylactic Acid (PLA)/Silica Nanocomposites

Surface-modified silica was incorporated into bio-based polylactic acid (PLA) to improve its performance. The modification by aminosilane on the silica was confirmed through FTIR (Fourier transform infrared) spectra. Following the aminosilane modification, polyethylene glycol methyl ether (PEGME) was grafted, via the aminosilane, on the silica to form the desired surface-modified silica (PEGME-silica). The grafting percentage of polyethylene glycol methyl ether was about 6.9 wt%. Unmodified silica, having underwent a similar treatment to maintain the same thermal history but without adding silane and PEGME, was also prepared. The PEGME-silica system had slightly higher tensile strength than the unmodified silica system, with a rheological study showing an enhanced polymer matrix-dispersed silica interaction and better dispersion in morphology observations being proposed as the cause. The dynamic storage modulus in the terminal zone was reduced for large amounts of highly dispersed surface-modified silica in comparison with unmodified silica. Tan δ decreased significantly with increasing unmodified silica contents in the low frequency region, resulting in solid-like behaviors. On the other hand, there was only a limited decrement for modified silica-filled samples in the corresponding ranges, especially for low dosages of the modified silica. The shear thinning phenomenon appeared to be more pronounced for unmodified silica at high silica content, but not for modified silica. To the best of our knowledge, this is the first report of the effect of polyethylene glycol methyl ether (PEGME)-modified nanosilica on the properties of PLA/silica nanocomposites prepared under a melt mixing process to illustrate the significance of surface modification via Cole–Cole plots.     

铜膜和铁膜污染物诱导熔石英表面损伤行为的对比研究

采用人工溅射的方式分别在熔石英基片上镀制了光学厚度相近的铜膜和铁膜污染物。研究了熔石英基底在355nm波长的激光损伤阈值。分别采用透射式光热透镜技术、椭偏仪、原子力显微镜和光学显微镜研究了两类薄膜的热吸收、膜层厚度、表面微观形貌以及激光辐照后薄膜的损伤形貌。实验结果表明：熔石英表面的金属膜状污染物均导致基片损伤阈值下降,位于前表面的污染物引起的损伤阈值下降更为严重,约为23％。两种污染物薄膜引起基底的损伤形貌、基底损伤阈值的下降幅度与薄膜的热吸收系数与微观结构有关。从热力学响应角度,结合损伤形貌对污染物诱导熔石英表面形貌的损伤机理进行了讨论。     

Interactions Between an Ionic Liquid and Silica,Silica and Silica,and Rubber and Silica and Their Effects on the Properties of Styrene-Butadiene Rubber Composites

An investigation of the effect of an ionic liquid, 1-butyl-3-methylimidazolium tetrafluoroborate (BMI), on the properties of silica reinforced styrene-butadiene rubber (SBR), aimed to correlate the interactions between the ionic liquid and silica, silica and silica, and silica and rubber with the macro-properties and microstructure of SBR and SBR/silica vulcanizates is described. The interaction between the ionic liquid and silica was characterized by differential scanning calorimetry (DSC) and Fourier transform infrared spectroscopy (FTIR), the interaction between silica and silica was characterized by a rubber processing analyzer (RPA), and the interaction between rubber and silica was characterized by the bound rubber content. The FTIR analysis revealed that BMI can react with the hydroxyl groups on the surface of silica, improving the compatibility between the rubber and silica. The RPA and bound rubber testing indicated that the interactions between silica and silica particles were weakened and the interaction between silica and rubber increased with the incorporation of BMI into the SBR rubber. The bound rubber content showed a maximum with a BMI content of 3 phr. At the same time, the dispersion of silica in SBR was improved with the incorporation of BMI. With the increase of BMI content, the curing rate was greatly improved and the crosslink density increased. BMI also increased the tensile strength and abrasion resistance of the SBR vulcanizates. Most important, the BMI significantly improved the dynamic properties of the rubber composites, especially the wet-skid resistance and rolling resistance. However, excessive BMI (beyond 3 phr) acted as a plasticizer and was detrimental to the mechanical properties, resulting in a decrease of tensile strength and abrasion resistance.     

Mechanical and Thermal Properties of Polypropylene/Silica Aerogel Composites

Polypropylene (PP) composites including various amounts of silica aerogel (SA) microparticles were prepared by melt mixing in an internal mixer. The morphology and microstructure of the prepared composites were investigated by scanning electron microscopy (SEM). Mechanical properties of the samples, including elastic modulus, tensile stress, elongation and stress at break, were measured by tensile tests. In addition, the other mechanical features, including Izod impact strength, hardness and wear resistance, were evaluated and then related to the structure of the PP/SA composites. Furthermore, the thermal characteristics of the composites, such as heat deflection temperature and thermal stability, were studied by thermal gravimetric analysis (TGA). The SEM photographs indicated the satisfactory SA particles dispersion for the compositions of 1% and 3% but agglomeration of the aerogels at higher SA contents. Since the composites became stiffer, the impact and tensile strength decreased. The addition of the SA to the PP matrix yielded harder samples with lower weight loss and coefficients of friction in wear tests. The TGA evaluations confirmed that the presence of SA promoted and upgraded the thermal stability and heat deflection temperature of PP. The thermal results proved the superior potential of PP as an insulator when the SA particles were added.