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The surface properties of fused silica (FS) change after H2O2 treatment, but the surface and subsurface damage behaviors and their mechanisms under various physical contact conditions have not been elucidated yet. This work investigated the effect of H2O2 treatment on mechanical and mechanochemical properties of FS surface. The results show that the hydrophilicity and adsorbed water film thickness of the FS surface increase with the concentration of H2O2 solution. The surface damage, nanowear, and subsurface deformation of FS caused by indentation increase with the concentration of H2O2 solution, while the nanohardness and reduced modulus decrease. Further analysis revealed that the water activity on the FS surface plays a critical role in reducing the mechanical and mechanochemical properties. In addition, the treatment with H2O2 solution on the FS surface shows a weakly corrosive effect, which implies the H2O2 treatment can be an alternative method to remove the surface defects on FS optics.

The optical performance of fused silica optics used in high-power lasers is known to depend not only on their surface damage resistance, but also on their surface quality. Previous studies have shown that good fused silica damage performance and surface quality can be achieved by the use of reactive ion etching (RIE), followed by HF-based wet shallow etching (3 μm). In this study, two kinds of HF-based etchants (aqueous HF and HF/NH4F solutions) were employed to investigate the effect of HF-based etching on the optical performance of reactive-ion-etched fused silica surfaces at various HF-based shallow etching depths. The results showed that the addition of NH4F to HF solution makes it possible to produce a high-quality optical surface with a high laser-induced damage threshold, which is strongly associated with the surface roughness and fluorescence defect density. Additionally, changing the HF-based etching depth over the range from 1 μm to 3 μm can affect the surface damage resistance and absorption performance of RIE-treated fused silica. The light-scattering results indicate that the point defect density plays an important role in the determination of the HF-based etching depth. Understanding these trends can enable the advantages of the combined technique of RIE and HF-based etching during the fabrication of high-quality fused silica optics.

A series of cleaning and etching experiments utilizing organic solvent or weak alkali solutions were performed on single-crystal silicon optics polished with different processes. Polishing-introduced fractured defects in the subsurface layer were systematically characterized using laser-induced scattering imaging and photothermal weak absorption imaging techniques. A white-light interferometer also measured the surface morphology and roughness of the samples to evaluate the surface quality of the optics. The results show that the organic solvent cleaning process can eliminate the surface contamination resulting from the environment and the near-surface polishing-introduced impurities but can not remove the fractured defects in the subsurface layer of the optics. By contrast, weak alkali solution can effectively expose the subsurface defects and decrease the concentration of the embedded absorbing impurities to some extent. The results also imply that the polishing process has a crucial effect on the surface quality (e.g., surface roughness and error) and optical performance (e.g., surface absorption) after the subsequent treatments such as cleaning or etching. The corresponding methodology of cleaning and characterization can serve as a predictive tool for evaluating the polishing level and laser damage resistance of the single-crystal silicon optics.

We investigate the role of each step in the combined treatment of reactive ion etching (RIE) and dynamic chemical etching (DCE) for improving the laser-induced damage resistance of fused silica optics. We employ various surface analytical methods to identify the possible damage precursors on fused silica surfaces treated with different processes (RIE, DCE, and their combination). The results show that RIE-induced defects, including F contamination, broken Si-O bonds, luminescence defects (i.e., NBOHCs and ODCs), and material densification, are potential factors that limit the improvement of laser-induced damage resistance of the optics. Although being capable of eliminating the above factors, the DCE treatment can achieve rough optical surface with masses of exposed scratches and pits which might serve as reservoirs of the deposits such as inorganic salts, thus limiting the further improvement in damage resistance of fused silica. The study guides us to a deep understanding of the laser-induced damage process in achieving fused silica optics with enhanced resistance to laser-induced damage by the combined treatment of RIE and DCE.

Fabrication of polymer composite fibers embedding ultra-long micro/nanowires via an iterative melt co-drawing and bundling technique is reported in this study. The poly(methyl methacrylate) (PMMA) porous array templates were prepared with section-cutting the PMMA/polystyrene (PS) (shell/core) composite fibers and dissolution of inner PS. The results showed that the PS cores or pores in the PMMA matrix are regularly arranged with hexagonal, and their diameter and spacing exhibits a uniform distribution. Especially, the core diameter can be precisely controlled from millimeter-scale to nanometer-scale by multi-step melt co-drawing. Based on the PMMA porous array templates, the Cu nanowires were successfully prepared by electrochemical deposition. Moreover, to fabricate PMMA ultra-long micro/nanowires, the composite fibers with converse shell/core component of PS/PMMA were initially prepared, and then the outer PS was dissolved. The obtained PMMA micro/nanowires were characterized with smooth complete orientation structure. The study provides an experimental basis for fabricating such polymer composite fibers, micro/nano porous array templates, and micro/nanowires with precise and controllable manner to meet the real application requirements.

Five novel azo dyes molecules with different intramolecular charge transfer (ICT) characters were synthesized and characterized. Their thermal stabilities were studied with thermogravimetric analysis (TGA). Their linear optical properties were investigated by Ultraviolet–visible (UV–Vis) and Fluorescence spectroscopy. △-Self-consistent-field density functional theoretical (SCF-DFT or simply △SCF) calculation and optical method were used to analyze the ICT strength of the azo Dyes 1, 2, 3, 4, 5, Disperse Red 1 (DR 1), DR 17 and DR 13. The fundamental gap, energy gaps (Eg) between HOMO and LUMO, optical gap falls down with the increase of the ICT strength. The third-order nonlinear optical (NLO) properties of azo dyes were investigated by Z-scan technique at the condition of 440 nm, 190 femtosecond, 20 Hz. The relationship between the third-order NLO properties and ICT character was discussed in detail. Going from dyes 1 → 2→3 → 4→5→DR 1→DR 17→DR 13, the Eg values decrease and the ICT strength increase. The third-order nonlinear susceptibility χ(3) and molecular second hyperpolarizability γ of the azo dyes are up to the order of 10−8 esu and 10−27 esu, respectively. The χ(3) and γ increase with the ICT strength. The Figures of Merit W » 1 and T « 1, meet the requirement of all-optical materials: W > 1 and T

The fabrication of geometry-controlled Cu microwires (CuMWs) using melt co-drawing and electrochemical deposition techniques is reported in this study; the resulting CuMWs have good surface quality and integrity. By designing and arranging the poly(methyl methacrylate) (PMMA)/polystyrene (PS) and PMMA fibres artificially, porous PMMA templates with different coding orders (e.g. “1 × 1”, “3 × 3”, “5 × 5”, and “7 × 7”) are created after multi-step drawing followed by the dissolution of the inner PS. With these templates, coding arrays of CuMWs with diameters of 2–10 μm are fabricated. The geometries of the obtained templates and CuMWs arrays are shown to be consistent with the design values. This new approach extends the types and quality of CuMWs and makes it possible to devise extremely complex array structures with micro or even nano dimensions for diverse optical applications such as spectral sensing, laser phased arrays, and photonic crystal fibres. Keywords: PMMA template, Melt co-drawing, Cu microwires, Coding array, Fibre

In this work, antireflective and superhydrophilic subwavelength nanostructured fused silica surfaces have been created by one-step, self-masking reactive ion etching (RIE). Bare fused silica substrates with no mask were placed in a RIE vacuum chamber, and then nanoscale fluorocarbon masks and subwavelength nanostructures (SWSs) automatically formed on these substrate after the appropriate RIE plasma process. The mechanism of plasma-induced self-masking SWS has been proposed in this paper. Plasma parameter effects on the morphology of SWS have been investigated to achieve perfect nanocone-like SWS for excellent antireflection, including process time, reactive gas, and pressure of the chamber. Optical properties, i.e., antireflection and optical scattering, were simulated by the finite difference time domain (FDTD) method. Calculated data agree well with the experiment results. The optimized SWS show ultrabroadband antireflective property (up to 99% from 500 to 1360 nm). An excellent improvement of transmission was achieved for the deep-ultraviolet (DUV) range. The proposed low-cost, highly efficient, and maskless method was applied to achieve ultrabroadband antireflective and superhydrophilic SWSs on a 100 mm optical window, which promises great potential for applications in the automotive industry, goggles, and optical devices.

Based on an advanced technology, randomly-aligned subwavelength structures (SWSs) were obtained by a metal-nanodot-induced one-step self-masking reactive-ion-etching process on a fused silica surface. Metal-fluoride (mainly ferrous-fluoride) nanodots induce and gather stable fluorocarbon polymer etching inhibitors in the reactive-ion-etching polymers as masks. Metal fluoride (mainly ferrous fluoride) is produced by the sputtering of argon plasma and the ion-enhanced chemical reaction of metal atoms. With an increase in CHF3/Ar gas flow ratio, the average height of the SWSs increases, the number of SWSs per specific area increases and then decreases, and the optical transmittance of visible light increases and then decreases. The optimum CHF3/Ar gas flow ratio for preparing SWSs is 1:5.

The damage behavior of fused silica optics induced by stimulated Brillouin scattering (SBS) was studied theoretically and experimentally based on a coupled-wave theory. The SBS-induced damage mechanism was systematically investigated by analyzing the evolutions of the Stokes-light intensity and induced stress as a function of laser pulse shape, thickness, and surface reflectance of the optics. The results show that the SBS-induced damage often occurs on the front surface of the fused silica optics. The Tophat beam has the most effect on an SBS-induced damage, followed by a focused Gaussian pulse. SBS effect is strongly thickness dependent, which is associated with the gain length. The SBS-induced damage can be efficiently suppressed by decreasing the surface reflection of the optics. Good agreements are obtained between the experimental and theoretical results, which strengthen our understanding of the damage mechanism of fused silica and provide a favorable reference for developing high-power laser systems.

The surface laser damage performance of fused silica optics is related to the distribution of surface defects. In this study, we used chemical etching assisted by ultrasound and magnetorheological finishing to modify defect distribution in a fused silica surface, resulting in fused silica samples with different laser damage performance. Non-destructive test methods such as UV laser-induced fluorescence imaging and photo-thermal deflection were used to characterize the surface defects that contribute to the absorption of UV laser radiation. Our results indicate that the two methods can quantitatively distinguish differences in the distribution of absorptive defects in fused silica samples subjected to different post-processing steps. The percentage of fluorescence defects and the weak absorption coefficient were strongly related to the damage threshold and damage density of fused silica optics, as confirmed by the correlation curves built from statistical analysis of experimental data. The results show that non-destructive evaluation methods such as laser-induced fluorescence and photo-thermal absorption can be effectively applied to estimate the damage performance of fused silica optics at 351 nm pulse laser radiation. This indirect evaluation method is effective for laser damage performance assessment of fused silica optics prior to utilization.

The simple yet efficient and versatile fabrication of colloidal crystals was investigated based on the solidification-induced colloidal crystallization process with particle/water suspension as precursor. The resulting colloidal crystals were constituted by crystal grains with sizes ranging from several tens of micrometers to a few millimeters. Each of the grains had a close-hexagonal array of colloids, which endowed the bulk colloidal crystal powders with some specific optical properties. The freezing of water was shown as the major driving force to form colloidal crystal grains, which supersaturated the solution with nanoparticles and thus induced the formation and growth of colloidal crystal seeds. This process is intrinsically different from those conventional methods based on shearing force, surface tension, columbic interaction or magnetic interaction, revealing a new strategy to fabricate colloidal crystals in a convenient and efficient way.

Buffered HF-based etching can effectively improve the laser damage resistance of the fused silica, but deep etching would cause the deteriorations in surface roughness and hardness, and decrease the laser-induced damage threshold. Capping a glass thin layer on the etched surface via plasma chemical vapor deposition in one step could overcome those deteriorations. We found that the deposition of the glass thin layer can further reduce the impurity element contamination and the PL intensity while retaining the low subsurface defect density as well as for the deeply etched sample. The surface quality, surface hardness and the laser damage resistance of the fused silica can be significantly improved by the glass thin layer, which reveals the potential application in high power laser facility.

Suppression of Fresnel reflection from diffraction grating surfaces is very important for many optical configurations. In this work, we propose a simple method to fabricate subwavelength structures on fused-silica transmission grating for optical antireflection. The fabrication is a one-step self-masking reaction ion etching (RIE) process without using any masks. According to effective medium theory, random cone-shaped nanopillars which are integrated on the grating surface can act as an antireflective layer. Effects of the nanostructures on the reflection and transmission properties of the grating were investigated through experiments and simulations. The nanostructure surface exhibited excellent antireflection performance, where the reflection of the grating surface was suppressed to zero over a wide range of incident angles. Results also revealed that the etching process can change the duty cycle of the grating, and thus the diffraction orders if there are oblique lateral walls. The simulation results were in good agreement with the experimental ones, which verified our physical comprehension and the corresponding numerical model. The proposed method would offer a low-cost and convenient way to improve the antireflective performance of transmission-diffractive elements.

HF-based wet deep etching is an effective method for improving the laser damage resistance of fused silica optics. However, the fact that the etching process involves HF reaction makes the operation very unsafe. Potassium hydroxide (KOH) has recently shown great potential to outperform the more commonly used HF-acid as an etchant for the damage resistance enhancement of fused silica optical surface. In this paper, we present a detailed investigation into how the KOH-based shallow etching process affects the polished surface of fused silica. The results show that KOH-based etching does a good job at exposing the subsurface damage and increasing the laser damage threshold of fused silica while keeping the surface roughness nearly unchanged. Potential factors that limit the further increase in surface damage threshold of fused silica are also delved. The study offers an exciting option for fabricating high-quality fused silica optics with shallow wet etching under higher safety conditions that cannot be achieved with conventional HF-based wet etching approaches.

In this paper we report a simple method to fabricate a novel subwavelength structure surface on fused silica substrate using one-step reactive ion etching with two-dimensional polystyrene colloidal crystals as masks. The etching process and the morphologies of the obtained structure are controlled. We show that the period of the obtained fused silica pillar-like arrays were determined by the initial polystyrene nanoparticle size. The height of pillar arrays can be adjusted by controlling the etching duration, which is proved to be of importance in tailoring the antireflection properties of subwavelength structures surface. The novel subwavelength structures surface exhibit excellent broadband antireflection properties, but the size of the pillar affects the antireflective properties in short wavelength region. We anticipate this method would offer a convenient and scalable way for inexpensive and high-efficiency high power laser field designs.

The antireflection (AR) performance and far-field transmittance, depending on the morphology and parameters of subwavelength structures (SWSs), have been investigated by a 3-D finite-difference time-domain (FDTD) method. It is found that far-field transmission characteristics are dominated mainly by period of SWSs. If the period is increased above 220 nm, the far-field transmittance rapidly decreases for a short-wavelength region. An effective and inexpensive method for fabricating disordered SWSs on fused silica has been demonstrated in this paper. An Au nanoscale island mask was formed by lower temperatures thermal dewetted at normal atmosphere. Then, a disordered SWS was fabricated by reactive ion etching (RIE). The average diameter of the Au nanoscale island was easily controlled by the thickness of Au thin films and annealing temperature. The etched depth and shape of fused silica SWSs depend additionally on RIE duration, thus achieving efficient AR characteristics. The measured data and calculated results obtained by the FDTD method exhibit reasonably similar tendencies. The optimized single-side fused silica SWS that is tapered on the tips leads to a significantly high transmissivity value of 96.2%. In addition, it exhibits a broadband AR property at a wavelength range of 400–1100 nm.

The ability to predict and control the influence of reaction ion etching process parameters on laser damage resistance of fused silica optical components is vital for their development in specialized applications such as inertial confinement fusion. In this study, a set of experiments was designed and performed to determine an optimized process condition by characterizing the evolution of the surface roughness and absorption of the fused silica samples treated at various gas flow rates. The macroscopic morphology, carbon concentration and laser damage resistance of the etched surface was measured. The optimized surface was obtained when the gas flow rate R (CHF 3 /(CHF 3 + Ar)) decreased down to 38.4%. With the optimized etch process, the presence of subsurface defects known to lead to laser damage initiation was removed and prevented. The C atomic concentration of the sample surface etched was decreased by 64.7%. The laser damage resistance increased dramatically; the average threshold fluence for damage initiation increased from 6.79 J/cm 2 to 8.99 J/cm 2 .

A facile method was proposed to enhance the laser damage performance of the fused silica optics by coating a PVA film on the rear surface of the optics. FDTD simulation result suggests that the PVA coating with suitable thickness can transfer the maximal electric field intensity from the rear surface to the interface between the coating and air, and reduce the electric field intensity of the rear surface remarkably. LIDT tests reveal that the LIDT of fused silica with PVA coating changed periodically with respect to the coating thickness, which agrees well with the tendency predicted by FDTD simulation. Finally, PVA coatings with a thickness of 60 nm and 300 nm can both improve the LIDT of AMP-treated fused silica by ~20%, which provide a potential to be applied in high power laser facility.

HF-based etching has been successful in mitigating damage precursors on the surface of fused silica optics used in high power lasers. However, wet etching generally leaves an etching trace leading to surface roughness, which seriously degrades laser beam quality (e.g., transmission loss and wave-front degradation). A way of addressing this issue is to apply plasma etching as a preprocessing step before HF etching, but so far very few studies have provided a practical scheme for engineering applications. In this work, we proposed a novel two-step scheme by combining reactive ion beam etching with dynamic chemical etching techniques. We demonstrate the combined scheme is capable of tracelessly mitigating the laser damage precursors on a fused silica surface. The 0% probability damage threshold obtained by combined etching is 1.4 times higher than that obtained by HF-based etching. The study opens a new approach towards high damage-resistant optics manufacturing and provides the potential possibility of exploring extreme interactions between high-power lasers and matter.

Hexagonally ordered arrays of polystyrene (PS) microspheres were prepared by a modified air-water self-assembly method. A detailed analysis of the air-water interface self-assembly process was conducted. Several parameters affect the quality of the monolayer colloidal crystals, i.e., the colloidal microsphere concentration on the latex, the surfactant concentration, the polystyrene microsphere diameter, the microsphere polydispersity, and the degree of sphericity of polystyrene microspheres. An abrupt change in surface tension was used to improve the quality of the monolayer colloidal crystal. Three typical microstructures, i.e., a cone, a pillar, and a binary structure were prepared by reactive-ion etching using a high-quality colloidal crystal mask. This study provides insight into the production of microsphere templates with flexible structures for large-area patterned materials.

In this Letter, an effective combined process of reaction ion etching (RIE) and dynamic chemical etching (DCE) is applied for significantly improving the damage resistance of fused silica optics, while minimizing the removal amount. By optimizing the combination process and removal depth, a near-perfect optical surface of fused silica with relatively low roughness (

Reactive ion etching (RIE) is crucial for fabricating high-quality fused silica optics since this technique can be used as a first step before dynamic chemical etching (DCE) for tracelessly removing the fractured defects in subsurface layer. The final quality of the optics is dramatically influenced by the plasma etching condition but still lacks sufficient information for practical application. In this work, combination of RIE and DCE was investigated deeply on polished fused silica surface by changing the gas type and flow rate. We show that the proper choice of fluorine-containing plasma condition during the RIE process allows the simultaneous occurrence of high surface quality and a low concentration of etching-introduced defects on fused silica. This leads to an ultrahigh laser-induced damage threshold at 355 nm while substantially keeping the surface roughness unchanged. This study paves the way for designing and developing a next-generation surface modification ability of high-quality fused silica with the great potential for high-power laser application.

Fluorinated ethylene propylene (FEP) film is an attractive candidate for mitigating target debris in high-power laser systems due to its remarkable advantages such as low cost, low absorption, and high damage threshold. However, the inert surface with bad wettability presents an enormous challenge to realize optical antireflection. In this Letter, we experimentally demonstrate that broadband antireflection of FEP film can be achieved through combining oxygen plasma treatment and solgel coating techniques. By optimizing the plasma treating time and withdrawal rate during the coating process, the treated FEP film has 4.7% enhanced transmittance compared to the untreated sample. In this case, transmittance over 99% with wide wave bands ranging from 600 to 950 nm is achieved. The mechanism of broadband antireflection was revealed by investigating the fluorocarbon groups on the FEP surface. The applicable wave band of antireflective FEP film can be designed at will by changing plasma-treating conditions, which could open up a new avenue in the field of laser debris mitigation.

The laser damage precursors in subsurface of fused silica (e.g. photosensitive impurities, scratches and redeposited silica compounds) were mitigated by mineral acid leaching and HF etching with multi-frequency ultrasonic agitation, respectively. The comparison of scratches morphology after static etching and high-frequency ultrasonic agitation etching was devoted in our case. And comparison of laser induce damage resistance of scratched and non-scratched fused silica surfaces after HF etching with high-frequency ultrasonic agitation were also investigated in this study. The global laser induce damage resistance was increased significantly after the laser damage precursors were mitigated in this case. The redeposition of reaction produce was avoided by involving multi-frequency ultrasonic and chemical leaching process. These methods made the increase of laser damage threshold more stable. In addition, there is no scratch related damage initiations found on the samples which were treated by Advanced Mitigation Process.

We investigate the interest of combined process of reactive ion etching (RIE) and dynamic chemical etching (DCE) as a final step after polishing to improve the laser damage resistance of fused silica optics at the wavelength of 355 nm. The investigation is carried out on the polished fused silica optics by changing the RIE depth while keeping the DCE depth fixed. We evidence that the combined etching process can effectively remove the damage precursors on the fused silica surface and thus improve its laser-induced damage threshold exceeding the level of the deep HF-etched surface. The effects of the combined etching depth on the surface roughness and surface error are also studied systematically. We show that the combined shallow etching can achieve better overall surface quality. Deeper etching will cause surface quality degradation of the fused silica optics, which is believed to be associated with the chemical etching during the combined process. Given that HF acid processing will degrade the surface quality of fused silica optics, the combined shallow etching appears as a pertinent alternative to HF-based deep etching.

The reactive ion etching (RIE) process of fused silica is often accompanied by surface contamination, which seriously degrades the ultraviolet laser damage performance of the optics. In this study, we find that the contamination behavior on the fused silica surface is very sensitive to the RIE process which can be significantly optimized by changing the plasma generating conditions such as discharge mode, etchant gas and electrode material. Additionally, an optimized RIE process is proposed to thoroughly remove polishing-introduced contamination and efficiently prevent the introduction of other contamination during the etching process. The research demonstrates the feasibility of improving the damage performance of fused silica optics by using the RIE technique.

This work presents a low-cost, simple, convenient, advanced technology to prepare large-area defect-free subwavelength structures (SWSs). SWSs were obtained by a metal-induced one-step self-masking RIE process on a fused-silica surface, in which metal-fluoride (mainly ferrous-fluoride) nanodots were used to induce and gather stable fluorocarbon polymer etching inhibitors in the RIE polymers as masks. The SWS growth processes are visible with an increase in etching time and some exhibit prominent broadband antireflective properties from the visible to the near-infrared wavelength range. Transmission in the 600-900-nm range increased from approximately 93% for the polished fused silica to above 99% for the double-side SWSs on fused silica. A theoretical simulation by a finite-difference time-domain method agreed well with the experiments. Moreover, the surface of the SWSs exhibits excellent superhydrophilic properties.

We demonstrate the effects of typical bulk defects in fused silica on the bulk damage threshold under nanosecond UV pulse in this study. A new test method is proposed to accurately evaluate laser induced bulk damage performance. The bulk bubble, hydroxyl, metal impurity, and weak absorption of the 355 nm laser are respectively characterized. The effects of bulk defects on bulk damage performance are analyzed statistically based on the correlation principle. For synthetic fused silica, metal impurities and hydroxyl have a weak correlation coefficient with the bulk damage threshold, while there is strong correlation between weak UV absorption and the bulk damage threshold. The influence of bulk damage threshold on surface damage performance is also discussed.