Reactive ion etching of GaAs with SiCl4: A residual damage and electrical investigation

The residual damage incurred by various SiCl₄ reactive ion etching (RIE) conditions was investigated by transmission electron microscopy (TEM), Raman spectroscopy, ion channeling, and electrical characterization methods. Lattice damage to depths greater than 100 nm was incurred in all of the RIE processing situations. The lowest power density, longest etch time RIE exhibited the lowest defect density, roughest surface morphology, and poorest quality GaAs regrowth. The highest power density, shortest etch time RIE displayed the highest defect density, smoothest surface morphology, and highest quality GaAs regrowth. The electrical measurements, Schottky diode characteristics, degraded with decreasing power density and increasing etch times. Overall, the characterization results suggest that the high power density, shortest etch time sample possesses the most desirable properties for device fabrication requirements.     

HfO2薄膜的离子束刻蚀特性研究

实验研究了HfO₂薄膜特性以及掩模材料AZ1350以Ar为工作气体下的离子束的刻蚀特性.给出了离子能量、离子束流密度和离子束入射角等因素与刻蚀速率的关系曲线,用最小二乘法拟合了上述因素与刻蚀斜率的函数关系方程;分析了光刻胶和基片在刻蚀过程中随刻蚀深度的变化对图形转移精度的影响,用AFM的Tapping模式测量了刻蚀前后HfO₂薄膜表面质量的变化.结果表明刻蚀速率与离子能量的平方根,及速流密度成正比,并随离子束入射角变化而变化;与刻蚀前相比,刻蚀工艺降低了因HfO₂薄膜刻蚀深度的增加引起图形转移精度下降,因此提高刻蚀选择比是获得高分辨率图形的前提.研究结果已应用到了在HfO₂/SiO₂多层膜衍射光栅的制作中.     

Local High-Frequency Magnetron Reactive-Ionic Quartz Etching

A high-frequency magnetron reactive-ion etching system for the high-speed quartz glass surface treatment is described. The scanning assembly of the magnetron is located in a separate chamber pumped down to a pressure of 10^–2 Pa. This ensures a highly uniform etching and a high magnetic induction on samples, making it possible to reduce the cathode thickness. The quartz etching was studied in SF₆, CF₄, and CHF₃ with the magnetron operation with and without scanning. The maximum etching rates of 1.6 m/min (with scanning) and 4.2 m/min (without scanning) were attained in CHF₃ with a 1-Pa pressure and 700-W discharge power. 150-m-depth 4-mm-diameter pits were obtained by the quartz etching without scanning. With an increase in the pit depth from 150 to 250 m, the etching rate was reduced from 4.2 to 2.5 m/min.     

The etching behaviour of silicon carbide compacts

A series of microstructural investigations has been undertaken in order to explore the reliability of particular etches in revealing microstructural detail in silicon carbide compacts. A series of specimens has been etched and examined following complete prior microstructural characterization by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and X-ray diffractometry techniques. In particular, the sensitivity of both a molten salt (KOH/KNO₃) etch and a commonly-used oxidizing electrolytic ‘colour’ etch to crystal purity, crystallographic orientation and polytypic structure has been established. The molten salt etch was found to be sensitive to grain boundaries and stacking disorder while the electrolytic etch was found to be primarily sensitive to local purity and crystallographic orientation. Neither etch appeared intrinsically polytype sensitive. Specifically, for the ‘colour’ etch, the p- or n-type character of impure regions appears critical in controlling etching behaviour; p-type impurities inhibiting, and n-type impurities enhancing, oxidation. The need to interpret etching behaviour in a manner consistent with the results obtained by a variety of other microstructural techniques will be emphasized.     

Chemical etching of natural fluorapatite crystals in acid solutions studied with the scanning electron microscope

Different aspects of the chemical etching process for natural fluorapatite (FAP) crystals in pure phosphoric acid solutions and for those with additives of Ca²⁺ and H₂SO₄ have been studied by means of the scanning electron microscope. The resulting experimental data obtained in the etching process are very sensitive to dissolving conditions, type of crystal face, and the presence or absence of any epitaxial coatings on the surface of dissolving crystals. It was found that the pyramidal crystal faces of the FAP have the highest dissolution rate value and, as a result, are not etched at all. The prism and pinacoid faces usually are covered by hexagonal etch pits under the same conditions. Additives of Ca²⁺ to the phosphoric acid solution result in transition from a chemical etching to a chemical polishing process, and additives of H₂SO₄ result in epitaxial coatings of CaSO₄· xH₂O (x = 0,0.5, 2) and shapeless pits formation.     

A technique for the preparation of cross-sectional TEM samples of ZnSe/GaAs heterostructures which eliminates process-induced defects

Cross-sectional transmission electron microscopy (TEM) sample preparation of ZnSe/GaAs epitaxial films is investigated. Conventional argon ion milling is shown to produce a high density (～ 5–8 × 10¹¹/cm²) of small (diameter ～ 60–80 Å) extended defects (stacking faults, microtwins, double positioning twins, etc.). In addition, transmission electron diffraction results indicate a thin ZnO layer can also occasionally form upon ion milling or electron-beam irradiation although the exact conditions for ZnO formation are not well understood. Conventional TEM (amplitude contrast) and high-resolution TEM (phase contrast) imaging in combination with transmission electron diffraction studies were performed to determine the optimum method of removing the ion milling related damage and ZnO layers during sample preparation. HF/HCl, NaOH/H₂O, H₂SO₄/H₂O₂/H₂O and Br₂/CH₃OH etching mixtures as well as low voltage argon or iodine ion milling were studied. A low energy (2 ke V) iodine or argon ion milling step was shown to remove the ZnO layer and reduced the density of the extended defects associated with Ar⁺ ion milling, but was unsuccessful in removing all of the defects. Auger electron spectroscopy results indicate residual iodine was either left on the surface or implanted beneath the surface during iodine ion milling. Etching the XTEM samples in HF/HCl was shown to be effective in removing the ZnO layer but had little or no effect on the ion milling induced defects. Etching the samples in a 0.5% Br₂/CH₃OH solution resulted in complete elimination of the ion milling induced extended defects including the residual defects associated with iodine ion milling. In addition the Br₂/CH₃OH etch produced the best surface morphology. Thus a brief (1–2 seconds) Br₂/CH₃OH etch after conventional preparation (argon ion milling) of cross-sectional ZnSe/GaAs TEM samples appears to be an inexpensive and superior alternative to iodine ion milling.     

Ultrastructural comparison of ion beam and radiofrequency plasma etching effects on biological tissue sections

Three dry etching techniques (Ar+ ion beam, O₂+ ion beam, O₂ radiofrequency electrodeless discharge) were compared with respect to preferential etching and damage to the ultrastructure of glutaraldehyde-fixed Epon-embedded frog skeletal muscle sections. SEM and TEM studies were performed on both unstained and stained (osmium tetroxide, uranyl acetate) sections. Etching effects were observed to differ for the various ion beam or plasma etching techniques. Whereas selective retention of electron dense structures (e.g. Z lines, nuclear heterochromatin) was observed for oxygen plasma etching, preferential etching of these components was observed using O₂+ ion beam bombardment. Selectively etched Z lines and etch-resistant nucleoli were observed for both reactive (O₂+) and inert (Ar+) ion beam sputtering after sufficiently high ion doses. The above suggest that selective etching under keV ion beam irradiation is related more to physical sputtering processes (momentum transfer) than to the chemical reactivity of the incident ion. Heavy metal post-fixation and staining had no qualitative effect on the nature of the selective etching phenomena. The above findings are significant in that they potentially influence both electron and ion microprobe measurements of etched biological specimens.     

Surface textures and process characteristics of the electrolytic photoetching of annealed AISI 304 stainless steel in hydrochloric acid

Electrolytic photoetching of AISI 304 stainless steel surfaces in 10% (w/w) hydrochloric acid has been studied. A surface texture value of 1.35 μm ($\text{R}{}_{\mathrm{a}}$) has been measured for a commercially acceptable rate of etch (10 μm/min). Comparisons of this etching system with FeCl₃-HCl-H₂O spray systems used in conventional photochemical machining have also been made     

湿法化学刻蚀技术处理抛光熔石英元件

为了提高熔石英元件的抗激光损伤能力,采用基于氢氟酸刻蚀的湿法化学技术去除元件内的激光损伤诱因。利用不同的氢氟酸溶液处理经氧化铈抛光的熔石英元件,并对元件的刻蚀速率、表面洁净度、粗糙度、透过率和激光损伤性能进行评价。研究结果表明,与传统的静态刻蚀相比,在质量分数为6%的氢氟酸刻蚀溶液中引入能量密度约为0.6 W/cm^2的兆声能量对元件的溶解速率和激光损伤性能没有明显的提升作用;化学刻蚀产生的沉积物对元件表面粗糙度和透过率均有不利影响,且沉积物比例与所用的刻蚀液成分和浓度密切相关;经质量分数6%或12%的纯氢氟酸溶液刻蚀(5±1)μm深度后,熔石英元件的激光损伤阈值相比于未刻蚀元件提升了约1.9倍;熔石英元件的激光损伤性能与表面粗糙度和透过率之间不是简单的线性关系,但激光损伤阈值较理想的元件(>20 J/cm^2@3ns)往往具有较光滑的表面,即表面粗糙度<2 nm,由此可以确定有利于熔石英元件激光损伤性能的刻蚀条件,并获得元件表面粗糙度的控制指标。     

Bonding performance of universal adhesives to er,cr:YSGG laser‐irradiated enamel

Universal adhesives have been recently introduced for use as self‐etch or etch‐and‐rinse adhesives depending on the dental substrate and clinical condition. However, their bonding effectiveness to laser‐irradiated enamel is still not well‐known. Thus, the aim of this study was to compare the shear bond strength (SBS) of universal adhesives (Single Bond Universal; Nova Compo‐B Plus) applied to Er,Cr:YSGG laser‐irradiated enamel with SBS of the same adhesives applied in self‐etch and acid‐etching modes, respectively. Crown segments of sixty bovine incisors were embedded into standardized acrylic blocks. Flattened enamel surfaces were prepared. Specimens were divided into six groups according to universal adhesives and application modes randomly (n = 10), as follows: Single Bond Universal/acid‐etching mode; Nova Compo‐B Plus/acid‐etching mode; Single Bond Universal/self‐etching mode; Nova Compo‐B Plus/self‐etching mode; and Single Bond Universal/Er,Cr:YSGG Laser‐etching mode; Nova Compo‐B Plus/Er,Cr:YSGG Laser‐etching mode. After surface treatments, universal adhesives were applied onto surfaces. SBS was determined after storage in water for 24 h using a universal testing machine with a crosshead speed of 0.5 mm min^?1. Failure modes were evaluated using a stereomicroscope. Data was analyzed using two‐way of analyses of variances (ANOVA) (p = 0.05). Two‐way ANOVA revealed that adhesive had no effect on SBS (p = 0.88), but application mode significantly influenced SBS (p = 0.00). Acid‐etching significantly increased SBS, whereas there are no significant differences between self‐etch mode and laser‐etching for both adhesives. The bond strength of universal adhesives may depend on application mode. Acid etching may significantly increase bond strength, while laser etching may provide similar bond strength when compared to self‐etch mode.     

Numerical study on the low density gas flows in a plasma etch reactor

The direct simulation Monte Carlo method is employed to predict the etch rate distribution on Al wafer for a chlorine feed gas flow. The etching process of an Al wafer in a plasma etch reactor is examined by simulating molecular collisions of reactant and product. The surface reaction on the Al wafer is simply modelled by one-step reaction: 3Cl₂+2Al → 2AlCl₃. The gas flow inside the reactor is compared for six different nozzle locations. The present numerical results show that the etch rate increases with the mass flow rate of source gas Cl₂. It is also shown that the flow field inside the reactor is significantly affected by the nozzle locations.     

Active application of primer acid on acid‐treated enamel: Influence on the bond effectiveness of self‐etch adhesives systems

Aim: Evaluate the composite‐to‐enamel bond after passive or active application of self‐etching primer systems on polished or pre‐etched enamel with phosphoric acid. Materials and Methods: Two self‐etch adhesives systems (SEAS) were used: Clearfil SE Bond and Easy Bond. Third human molars were divided into 8 groups (N = 10). The crown of each tooth was sectioned into halves and the mesial/distal surfaces were used. The adhesives were actively or passively applied on enamel with or without prior phosphoric‐acid etching. Resin composite cylinders were built after adhesive application. After stored in relative humidity for 24 hr/37°C the specimens were subjected to microshear test in universal testing a machine at a crosshead speed of 0.5 mm/minute. The results were analyzed with three‐way ANOVA and the Tukey test. The enamel‐etching pattern was evaluated under SEM. Results: The 2‐step SEAS system presented significantly higher adhesive bond strength means (47.37 MPa) than the 1‐step (36.87 MPa). A poor enamel‐ etching pattern was observed in active mode showing irregular and short resin tags, however there was not compromised the bond strength. Conclusion: Active or passive application produced similar values of bond strength to enamel regardless of enamel pretreatment and type of SEAS.     

Micromorphology analysis and bond strength of two adhesives to Er,Cr:YSGG laser‐prepared vs. Bur‐prepared fluorosed enamel

Preservation of enamel during composite veneer restorations of fluorosed teeth could be achieved by conservative preparation with Erbium lasers. This study evaluated the effect of fluorosed enamel preparation with Er,Cr:YSGG vs. conventional diamond bur on the micromorphology and bond strength of a self‐etch and an etch‐and‐rinse adhesives. Er,Cr:YSGG laser or diamond bur preparation was performed on the flattened midbuccal surfaces of 70 extracted human premolars with moderate fluorosis (according to Thylstrup and Fejerskov index, TFI = 4–6). Adper Single Bond (SB) with acid etching for 20 or 40 s and Clearfil SE Bond (SEB) alone or with additional etching was applied in four laser groups. The same adhesive procedures were used in three bur groups except for 40 s of etching along with SB. After restoration, microshear bond strength was measured (MPa). Data were analyzed using ANOVA and Tamhane tests (α = 0.05). Six additional specimens were differently prepared and conditioned for scanning electron microscopy evaluation. The highest and lowest bond strengths were obtained for bur‐prepared/SB (39.5) and laser‐prepared/SEB (16.9), respectively, with a significant difference (P = 0.001). The different adhesive procedures used associated to two adhesives exhibited insignificantly lower bonding in laser‐prepared groups compared to bur‐prepared ones (P > 0.05), with the exception of additional etching/SEB, which bonded significantly higher to bur‐prepared (36.4) than to laser‐prepared enamel (18.7, P = 0.04). Morphological analyses revealed a delicate etch pattern with exposed enamel prisms on laser‐prepared fluorosed enamel after acid etching and less microretentive pattern after self‐etching primer. The etch‐and‐rinse adhesive was preferred in the laser‐prepared fluorosed enamel in terms of bonding performance. Microsc. Res. Tech. 77:779–784, 2014. © 2014 Wiley Periodicals, Inc.     

Dislocations in CdTe heteroepitaxial structures on GaAs(301) and Si(301) substrates

Initial stages of ZnTe growth on GaAs(301) and Si(301) substrates by the method of molecular beam epitaxy are investigated by means of in situ one-wave ellipsometry. Layer-by-layer growth of the ZnTe film is observed on GaAs(301) substrates, whereas 3D nucleation occurs during epitaxy on Si(301) substrates. Misfit dislocations (MDs) are inserted into the ZnTe film during the growth of the first monolayers. Owing to MDs, the film lattice turns with respect to the substrate lattice, which is confirmed by X-ray measurements. Threading segments of MDs in CdTe/ZnTe/GaAs(301) and CdTe/ZnTe/Si(301) heterostructures are subjected to etching. The etch dislocation pits are found to have different shapes, which testifies to different types of threading dislocations. In the case of layer-by-layer etching, the dislocation density is found to increase inward the CdTe film, which testifies to annihilation of dislocations in the course of growth of CdTe films. The dislocation annihilation rate is higher in films grown on GaAs(301) than in those grown on Si(301). A possible reason is the higher mobility of dislocations in CdTe films on GaAs(301) substrates.     

Comparison of total‐etch,self‐etch,and selective etching techniques on class V composite restorations prepared by Er:YAG laser and bur: a scanning electron microscopy study

The purpose of this study was to compare total‐etch, self‐etch, and selective etching techniques on the marginal microleakage of Class V composite restorations prepared by Er:YAG laser and bur. Class V cavities prepared on both buccal and lingual surfaces of 30 premolars by Er:YAG laser or bur and divided into six groups. The occlusal margins were in enamel, and the cervical margins were in cementum. Group‐1: bur preparation(bp)+Adper Single Bond 2 (ASB)+Filtek Z550 (FZ); Group‐2: laser preparation(lp)+(ASB)+(FZ); Group‐3: bp + Clearfil S3 Bond Plus (CSBP)+(FZ); Group‐4: lp+(CSBP) (FZ); Group‐5: bp + acid etching+(CSBP)+(FZ); Group‐6: lp + acid etching+(CSBP)+(FZ). All teeth were stored in distilled water at 37°C for 24 hr, and then thermocycled 1000 times (5–55°C). Five teeth from each group were chosen for the microleakage investigation, and two teeth for the scanning electron microscope evaluation. Teeth which were prepared for the microleakage test were immersed in .5% methylene blue dye for 24 hr. After immersion, the teeth were sectioned and observed under a stereomicroscope for dye penetration. Data were analyzed using Kruskal–Wallis and Mann–Whitney U tests (p < .05). More microleakage was observed in the cervical regions compared to the occlusal regions in Groups 3, 5, and 6, respectively (p < .05). There is no statistically significant difference in Groups 1, 2, and 4, in terms of cervical regions versus occlusal regions (p > .05). No significant differences were observed among any groups in terms of occlusal and cervical surfaces, separately (p > .05). Different etching techniques did not influence microleakage of Class V restorations prepared by Er:YAG laser and bur.     

图形化蓝宝石衬底干法刻蚀工艺研究

为了缩短刻蚀时间以及提高发光二极管（LEDs）的发光性能,针对添加刻蚀辅助气体三氟甲烷（CHF3）的干法刻蚀工艺进行了研究。采用感应耦合等离子（ICP）干法刻蚀技术并通过正交试验研究了偏压功率、CHF3流量、自动压力控制蝶阀开合度（APC）对刻蚀速率和选择比的影响。试验结果表明：当偏压功率、CHF3流量和APC分别为350W、15 sccm和55%时,制程工艺有着更大的刻蚀选择比和蓝宝石刻蚀速率。使用最佳工艺参数制备出了大尺寸、高占空比、小弧度图形化蓝宝石衬底（PSS）,与常规PSS相比,优化后的工艺参数制得的PSS高度增加了5.6%、占空比提高了4.6%。     

超声技术在石英光纤腐蚀中的运用

为了获得光滑的腐蚀光纤表面并精确管理光纤的腐蚀直径,采用自行设计的超声腐蚀系统,在质量百分比浓度为12.5％的氢氟酸(HF)溶液中研究了超声功率和腐蚀温度对石英光纤包层、纤芯腐蚀速率以及腐蚀后光纤表面形貌的影响.研究表明:在HF溶液中,超声扰动有利于提高光纤的腐蚀速率,光纤腐蚀速率与腐蚀时间呈非线性关系,腐蚀表面随着腐蚀的进行越来越粗糙.基于研究结果,进一步采用质量百分比浓度为12.5％的HF溶液和25％的NH4OH溶液配制了缓冲氢氟酸(BHF)溶液,探讨了光纤腐蚀速率及表面形貌的变化,结果表明:在V(HF)∶V(NH4OH)=2的BHF溶液中,当超声功率为165 W、腐蚀温度为40℃时,可获得光滑的腐蚀光纤表面和腐蚀速率与腐蚀时间的线性关系.     

VO2/GaAs异质结的制备及其光电特性研究

采用直流磁控溅射和后退火氧化工艺在p型GaAs单晶衬底上成功制备了n-VO_2/pGaAs异质结,研究了不同退火温度和退火时间对VO_2/GaAs异质结性能的影响,并分析其结晶取向、化学组分、膜层质量以及光电特性。结果表明,在退火时间2 h和退火温度693 K下能得到相变性能最佳的VO_2薄膜,相变前后电阻变化约2个数量级。VO_2/GaAs异质结在308 K、318 K和328 K温度下具有较好的整流特性,对应温度下的阈值跳变电压分别为6.9 V、6.6 V和6.2 V,该结果为基于VO_2相变特性的异质结光电器件的设计与应用提供了可行性。     

Dentin bond strength and nanoleakage of the adhesive interface after intracoronal bleaching

This study evaluated dentin bond strength (BS) and nanoleakage of non‐ and pre‐etched dentin immediately (T₀,), 7 days (T₇), and 14 days (T₁₄) after bleaching. Bovine incisors (150) were selected and half of them submitted to intrapulpal dentin etching (e). Non‐ and pre‐etched dentin were subjected to the following (n = 15): no bleaching/control (C); 35% carbamide peroxide (CP); 35% hydrogen peroxide (35% HP); 25% hydrogen peroxide (25% HP); and sodium perborate (SP). Bleaching agents were applied to the pulp chamber four times within a 72‐h interval. Afterwards, pulp chamber dentin was prepared for the BS test at different evaluation times (n = 5): T₀, T₇, and T₁₄. Composite blocks were built on pulp chamber and sectioned in slices. Slices were reduced to an hour‐glass shape with a cross‐sectional area of 0.8 mm² and submitted to microtensile BS test. Two additional specimens for each group were prepared for nanoleakage evaluation by transmission electron microscopy (TEM). Results were analyzed by ANOVA (two‐way) and Dunnett's test (p < .05). BS decreased immediately after intracoronal bleaching for both sound and pre‐etched dentin (p < .05). At T₁₄, the BS of non‐etched bleached dentin increased for all groups, whereas the pre‐etched SPe group presented BS similar to the Ce. Nanoleakage within the hybrid layer was perceptible immediately after bleaching, although a decrease in nanoleakage was observed for all groups at T₁₄. Adhesive restorations should be performed 7–14 days after bleaching, according to the bleaching agent used. Intracoronal bleaching should be performed preferably with sodium perborate if previous dentin etching is applied.     

Structure, Mechanical, and Tribological Properties of MoS2/a-C:H Composite Films

A series of hydrogenated amorphous carbon (a-C:H) films doped with molybdenum disulfide (MoS₂) were deposited by medium frequency unbalanced magnetron sputtering with mixed Ar/CH₄ gases of different volume ratios as the source gases. The effects of Ar/CH₄ ratio on morphology, microstructure, mechanical, and tribological properties of the MoS₂/a-C:H composite films were investigated. Results show that the content of MoS₂ in the as-deposited films decreases with the decreasing Ar/CH₄ ratio, and the highest Ar/CH₄ ratio favors the formation of nanostructured films. Besides, the hardness and internal stress of the composite films first decrease and then increase with decreasing Ar/CH₄ ratio. Furthermore, the film deposited at the highest Ar/CH₄ ratio exhibits excellent antiwear ability in all test environments and shows promising potential as a solid lubricating film in aviation and space industries.