非晶熔石英表面等离子体刻蚀过程 中的表面晶化研究

本工作采用电子回旋共振(ECR)低压等离子体刻蚀技术, 刻蚀非晶熔石英表面. Ar/CF₄为反应气体刻蚀后再经O等离子体钝化, 非晶熔石英表面出现晶化现象. 晶化层约几百纳米厚. Ar/CF₄在ECR的电磁场作用下产生F离子与C离子, F离子使熔石英表面的Si-O共价键断裂, 并释放出O离子. C离子与O离子迅速键合生成CO₂, 而被断键的Si原子与四个F原子键合生成气态SiF₄. 熔石英原始表面被去除的同时, 在新的表面留下大量不饱和Si原子. 不饱和Si原子在高温条件下被O等离子钝化, 形成结晶态α 方石英.     

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。     

超声波辅助酸蚀提高熔石英损伤阈值

为了提高熔石英元件表面抗激光损伤阈值,利用超声波辅助HF酸研究平滑光学元件表面缺陷形貌和去除刻蚀后残留物效果,通过扫描电子显微镜电镜和原子力显微镜记录表面形貌结构,以及单脉冲激光辐照测试抗损伤阈值确定实验参数。研究表明,超声波场的引入能催化HF酸的刻蚀速率、提高钝化效果并且更易剥离嵌入的亚μm级杂质粒子。经过实验测试,获得了熔石英类元件相匹配的超声辅助HF酸刻蚀实验参数,研究结果对应用超声波辅助HF酸研究熔石英表面抗激光损伤有重要意义。     

同步辐射Laminar光栅的研制

采用全息离子束刻蚀和反应离子刻蚀相结合的新工艺 ,在熔石英基片上成功地刻蚀出 2 0 0l/mm、线空比 4:6、槽深 70nm、刻划面积 60× 2 0mm2 的浅槽矩形Laminar光栅。对改进光栅线条粗糙度和线空比的方法进行了系统的研究。这一新工艺相对简单 ,降低了对干涉系统光学元件和全息曝光显影的严格要求     

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%。     

化学刻蚀过程中熔石英表面沉积物的形成及其对激光损伤的影响

化学刻蚀是提升熔石英光学元件抗激光损伤性能的重要后处理技术之一,但刻蚀后熔石英表面附着的沉积物对其表面质量、透射性能和抗激光损伤性能有很大影响。使用光学显微镜和原子力显微镜表征了化学刻蚀后附着于熔石英表面的沉积物的微观形貌,并分析了其形成机理;X射线能谱分析表明化学刻蚀后熔石英表面沉积物主要由Fe,Ni,Al等元素的金属盐组成。损伤阈值测试结果表明熔石英表面高密度沉积物区域的损伤阈值明显低于非沉积物区域,沉积物对熔石英光学元件的抗激光损伤性能产生严重影响,它们是诱导熔石英激光损伤的前驱体。     

离子源工艺参数对BCB胶刻蚀速率和表面粗糙度的影响

为了研究离子束刻蚀抛光过程中离子源工艺参数对刻蚀速率及表面粗糙度的影响,采用微波离子源为刻蚀离子源,以BCB胶为主要研究对象,研究了离子束能量、离子束电流、氩气流量、氧气流量对BCB胶刻蚀速率及表面粗糙度的影响,获得了离子源工艺参数与刻蚀速率及表面粗糙度演变的关系。研究结果表明,离子束能量在从400 eV增大到800 eV的过程中,刻蚀速率不断增大,从3.2 nm/min增大到16.6 nm/min;离子束流密度在从15 mA增大到35 mA的过程中,刻蚀速率不断增大,从1.1 nm/min增大到2.2 nm/min;工作气体中氧气流量从2 mL/min增大到10 mL/min的过程中,刻蚀速率会整体增大,在8 mL/min处略有下降。表面粗糙度变化不大,可以控制在1.8 nm以下。     

发射光谱法在等离子体刻蚀废气微量F元素检测中的应用研究

以CF4Ar为等离子体刻蚀废气的模拟气体 ,利用发射光谱法分析F。含氟废气中 F原子的发射光谱在6 0 0— 80 0 nm波段内的谱线为 6 97.5 nm和 739.5 nm。研究了电感耦合等离子体放电时射频功率对F元素检测的影响 ,表明提高射频功率可降低 F元素检出限。     

发射光谱法研究CaO对等离子体刻蚀废气的吸收作用

以 CF4/ Ar作为等离子体刻蚀废气的模拟气体 ,经电感耦合等离子放电之后 ,通过 Ca O固体粉末进行废气的吸收 ,测得吸收废气的 Ca O的发射光谱。与模拟刻蚀废气光谱比较可知 ,Ca O可除去废气中70 %的 F元素 ,并给出了未能全部清除的原因。     

基于磁控溅射和ICP刻蚀的RB-SiC表面平坦化工艺

采用射频磁控溅射技术在RB-SiC表面沉积Si平坦化层,通过正交试验研究了射频功率、Ar流量和工作气压三个因素对薄膜表面质量和形貌的影响规律,以获取最佳的薄膜沉积参数.射频功率120 W、工作气压1.2Pa和Ar流量40sccm条件下获得了最佳质量的平坦化样品,利用电感耦合等离子体对平坦化膜层进行刻蚀抛光,通过Lambda950分光光度计测试不同工艺阶段样品表面的反射率.结果表明,相比于未处理的RB-SiC初始样品,经过平坦化和等离子体刻蚀的样品表面粗糙度标准差值由1.819nm减小至0.919nm,样品表面反射率相应地提高了2%.由此说明射频磁控溅射平坦化沉积与电感耦合等离子体刻蚀的组合工艺可实现RB-SiC表面的高质量加工.     

Elucidating surface properties of dry-etched ZnO using H2/CH4 and H2/CH4/Ar plasma

This paper reports a study of reactive ion etching (RIE) of n-ZnO in H₂/CH₄ and H₂/CH₄/Ar gas mixtures. Variables in the experiment were gas flow ratios, radio-frequency (rf) plasma power, and total pressure. Structural and electrical parameters of the etched surfaces and films were determined. Both the highest surface roughness and highest etching rate of ZnO films were obtained with a maximum rf power of 300 W, but at different gas flow ratios and working pressures. These results were expected because increasing the rf power increased the bond-breaking efficiency of ZnO. The highest degree of surface roughness was a result of pure physical etching by H₂ gas without mixed CH₄ gas. The highest etching rate was obtained from physical etching of H₂/Ar species associated with chemical reaction of CH₄ species. Additionally, the H₂/CH₄/Ar plasma treatment drastically decreased the specific contact and sheet resistance of the ZnO films. These results indicated that etching the ZnO film had roughened the surface and reduced its resistivity to ohmic contact, supporting the application of a roughened transparent contact layer (TCL) in light-emitting diodes (LEDs).     

Dry etching of bulk single-crystal ZnO in CH4/H2-based plasma chemistries

The effect of inert gas additive (He, Ar, Xe) to CH₄/H₂ discharges for dry etching of single crystal ZnO was examined. The etch rates were higher with Ar or Xe addition, compared to He but in all cases the CH₄/H₂-based mixtures showed little or no enhancement over pure physical sputtering under the same conditions. The etched surface morphologies were smooth, independent of the inert gas additive species and the Zn/O ratio in the near-surface region decreases as the mass number of the additive species increases, suggesting preferential sputtering of O. The plasma etching improved the band-edge photoluminescence intensity from the ZnO for the range of ion energies used here (290-355 eV), due possibly to removal of surface contamination layer.     

High-density plasma etching of indium-zinc oxide films in Ar/Cl2 and Ar/CH4/H2 chemistries

The dry etching characteristics of transparent and conductive indium-zinc oxide (IZO) films have been investigated using an inductively coupled high-density plasma. While the Cl₂-based plasma mixture showed little enhancement over physical sputtering in a pure argon atmosphere, the CH₄/H₂/Ar chemistry produced an increase of the IZO etch rate. On the other hand, the surface morphology of IZO films after etching in Ar and Ar/Cl₂ discharges is smooth, whereas that after etching in CH₄/H₂/Ar presents particle-like features resulting from the preferential desorption of In- and O-containing products. Etching in CH₄/H₂/Ar also produces formation of a Zn-rich surface layer, whose thickness (∼40 nm) is well-above the expected range of incident ions in the material (∼1 nm). Such alteration of the IZO layer after etching in CH₄/H₂/Ar plasmas is expected to have a significant impact on the transparent electrode properties in optoelectronic device fabrication.     

Comparison of CH4/H2 and C2H6/H2 inductively coupled plasma etching of ZnO

CH₄/H₂-based discharges are attractive for dry etching of single crystal ZnO because of their non-corrosive nature. We show that substitution of C₂H₆ for CH₄ increases the ZnO etch rate by approximately a factor of 2 both with and without any inert gas additive. The C₂H₆/H₂/Ar mixture provides a strong enhancement over pure Ar sputtering, in sharp contrast to the case of CH₄/H₂/Ar. The threshold ion energy for initiating etching is 42.4 eV for C₂H₆/H₂/Ar and 59.8 eV for CH₄/H₂/Ar. The etched surface morphologies were smooth, independent of the chemistry and the Zn/O ratio in the near-surface region was unchanged within experimental error after etching with both chemistries. The plasma etching improved the band-edge photoluminescence intensity and suppressed the deep level emission from the bulk ZnO under our conditions, due possibly to removal of surface contamination layer.     

HfO2顶层多层介质膜脉宽压缩光栅的离子束刻蚀

多层介质膜光栅是高功率激光系统的关键光学元件. 为了满足国内强激光系统的迫切需求,首先利用考夫曼型离子束刻蚀机开展了HfO₂顶层多层介质膜脉宽压缩光栅的离子束刻蚀实验研究. 采用纯Ar及Ar和CHF₃混合气体作为工作气体进行离子束刻蚀实验,获得了优化的离子源工作参数. 结果表明,与纯Ar离子束刻蚀相比,Ar和CHF₃混合气体离子束刻蚀时的HfO₂/光刻胶的选择比大. HfO₂的离子束刻蚀过程中再沉积效应明显,导致刻蚀光栅占宽比变大. 根据刻蚀速率分布制作的掩模遮挡板可以提高刻蚀速率均匀性,及时清洗离子源和更换灯丝,可保证刻蚀工艺的重复性. 利用上述技术已成功研制出多块最大尺寸为80 mm×150 mm、线密度1480线/mm、平均衍射效率大于95%的HfO₂顶层多层介质膜脉宽压缩光栅. 实验结果与理论设计一致,为大口径多层介质膜脉宽压缩光栅的离子束刻蚀提供了有益参考. 关键词： 光栅 多层介质膜 离子束刻蚀     

Argon-dominated plasma beam generated by filtered vacuum arc and its substrate etching

A new technique to etch a substrate as a pre-treatment prior to functional film deposition was developed using a filtered vacuum arc plasma. An Ar-dominated plasma beam was generated from filtered carbon arc plasma by introducing appropriate flow rate of Ar gas in a T-shape filtered arc deposition (T-FAD) system. The radiation spectra emitted from the filtered plasma beam in front of a substrate table were measured. The substrate was etched by the Ar-dominated plasma beam. The principal results are summarized as follows. At a high flow rate of Ar gas (50 ml/min), when the bias was applied to the substrate, the plasma was attracted toward the substrate table and the substrate was well etched without film formation on the substrate. Super hard alloy (WC), bearing steel (SUJ2), and Si wafer were etched by the Ar-dominated plasma beam. The etching rate was dependent on the kind of substrate. The roughness of the substrate increased, when the etching rate was high. A pulse bias etched the substrate without roughening the substrate surface excessively.     

Dry etching of zinc-oxide and indium-zinc-oxide in IBr and BI3 plasma chemistries

The dry etching characteristics of bulk single-crystal zinc-oxide (ZnO) and RF-sputtered indium-zinc-oxide (IZO) films have been investigated using an inductively coupled high-density plasma in Ar/IBr and Ar/BI₃. In both plasma chemistries, the etch rate of ZnO is very similar to that of IZO, which indicates that zinc and indium atoms are driven by a similar plasma etching dynamics. IBr and BI₃-based plasmas show no enhancement of the etch rate over pure physical sputtering under the same experimental conditions. The etched surface morphologies are smooth, independent of the discharge chemistry. From Auger electron spectroscopy, it is found that the near-surface stoichiometry is unchanged within experimental error, indicating a low degree of plasma-induced damage.     

Dry etching characteristics of GaN for blue/green light-emitting diode fabrication

The etch rates, surface morphology and sidewall profiles of features formed in GaN/InGaN/AlGaN multiple quantum well light-emitting diodes by Cl₂-based dry etching are reported. The chlorine provides an enhancement in etch rate of over a factor of 40 relative to the physical etching provided by Ar and the etching is reactant-limited until chlorine gas flow rates of at least 50 standard cubic centimeters per minute. Mesa sidewall profile angle control is possible using a combination of Cl₂/Ar plasma chemistry and SiO₂ mask. N-face GaN is found to etch faster than Ga-face surfaces under the same conditions. Patterning of the sapphire substrate for improved light extraction is also possible using the same plasma chemistry.     

Atomic force microscopy investigation of surface roughness generated between SiO2 micro-pits in CHF3/Ar plasma

The present paper investigates the surface roughness generated by reactive ion etching (RIE) on the location between silicon dioxide (SiO₂) micro-pits structures. The micro-pit pattern on polymethyl methacrylate (PMMA) mask was created by an electron beam lithography tool. By using PMMA as a polymer resist mask layer for pattern transfer in RIE process, the carbon (C) content in etching process is increased, which leads to decrease of F/C ratio and causes domination of polymerization reactions. This leads to high surface roughness via self-organized nanostructure features generated on SiO₂ surface which was analyzed using atomic force microscopy (AFM) technique. The etching chemistry of CHF₃ plasma on PMMA masking layer and SiO₂ is analyzed to explain the polymerization. The surface root-mean-square (RMS) roughness below 1 nm was achieved by decreasing the RF power to 150 W and process pressure lower than 10 mTorr.     

使用发射光谱对H2稀释情况下的感应耦合H2/C4F8等离子体中碳氟基团的研究

在射频输入功率为400W，气压为0.8Pa的条件下，使用光强标定的发射光谱方法研究了感应耦合H₂/C₄F₈等离子体中CF, CF₂, H和F基团的相对密度随流量比R=H₂/(H₂+C₄F₈)的变化情况，而HF基团相对密度的变化由四级质谱仪探测得到。结果表明等离子体活性先随着R的增加而升高，然后随着R的进一步增加而下降。在流量比从0逐渐上升到0.625的过程中，CF和CF₂基团的相对密度不断降低。实验中测得的CF基团的相对密度[CF]与理论计算得到的[CF]有很好的一致性说明了电子与CF2基团的碰撞反应是CF基团产生的主要原因。文中还讨论了HF基团。