Sapphire Window Research Articles

Design and application of a high-pressure combustion chamber for studying propellant flames with laser diagnostics.

This manuscript presents the design and initial application of a high-pressure combustion chamber (HPCC). The HPCC exhibits several unique design attributes to enable high-fidelity studies of propellant-combustion physics at high pressures. The HPCC employs a flangeless and weldless design to provide a compact, easy to access, and relatively light weight (for its size and pressure capability) test chamber. It has a cylindrical test volume of 13.1 L and is capable of operating at pressures from approximately 0.4 mbar to 200 bar. The vessel is equipped with a ZnSe window to enable the laser ignition of propellants and energetic materials and 4 sapphire windows (2″ diameter and 4″ × 2″ slots) to enable the use of multiple optical diagnostics spanning the ultraviolet to mid-infrared. The sapphire windows are mounted in plugs with adjustable length to bring the windows inside of the test volume and facilitate line-of-sight optical measurements. The vessel can be accessed from the top and bottom via removable 5″ diameter plugs, and the bottom plug can be modified to enable studies of gaseous jets and flames. Some of the HPCC's testing capabilities are demonstrated via high-speed IR imaging and laser-absorption-spectroscopy measurements of temperature and CO in laser-ignited HMX (i.e., 1,3,5,7-tetranitro-1,3,5,7-tetrazoctane) flames at pressures from 2 to 25 bar.

Effective sapphire repellency treatment to reduce fouling of a focused beam reflectance measurement (FBRM) probe in bituminous systems

AbstractThe use of a focused beam reflectance measurement (FBRM) probe to track the chord length distribution dynamics in a bituminous system can be very challenging. Material coats the sapphire window of the probe and the quality of the data is compromised. The fouling index is a parameter used to assess the quality of the FBRM data. It is provided by the software and is the percentage similarity between two consecutive scans of the instrument, indicating how much of the reading has not changed due to material that is stuck to the optical window. When the FBRM was used in bitumen froth, the fouling index was higher than 90 %. In this work the significant reduction in fouling achieved with a sapphire repellency treatment is presented. The reduction in fouling was sufficient to detect broad trends in the FBRM data that will be used in future studies but was not sufficient to ensure quantitative measurement of the chord length distribution.

In-Cylinder GDI Soot via Visualization and Time-Resolved Total Cylinder Sampling

<div class="section abstract"><div class="htmlview paragraph">For better understanding, model development and its validation of in-cylinder soot formation processes of Gasoline Direct Injection (GDI) engines, crank-angle-resolved mass and size distribution of in-cylinder soot during a GDI combustion cycle were investigated via optical measurements and total cylinder sampling technique in an optically accessible Rapid Compression and Expansion Machine (RCEM). A direct-injection, spark-ignited and single-shot combustion event was achieved in the RCEM operated with engine speed 600 rpm, compression ratio 9.0, equivalence ratio 0.9 and natural aspiration. A three-component (iso-octane 65%, n-heptane 10%, toluene 25%) gasoline surrogate fuel and a multi-hole injector shared within the Japanese SIP Innovative Combustion Technology research program were used. As for the optical measurements, two-color method and laser/LED-based Diffused Back Illumination (DBI) high-speed imaging through sapphire windows on the cylinder head and the flat-top piston provided time-sequential in-cylinder soot mass. As for the total cylinder sampling, filter gravimetry and Portable Aerosol Mobility Spectrometer (PAMS) measurements of total-cylinder soot-laden gas provided crank-angle-resolved in-cylinder soot mass and size distribution. The total cylinder sampling was realized by replacing the cylinder head window with a stainless-steel diaphragm, rupturing the diaphragm at an arbitrary crank angle during combustion and rapidly expanding the total-cylinder soot-laden gas to effectively freeze secondary reactions and agglomeration of soot particles. The in-cylinder soot mass obtained by the above mentioned four different methods showed reasonable agreement each other both in increasing trend during combustion and quantitative soot mass. Measured variation of soot size distribution during combustion indicates that formation and agglomeration of soot are simultaneously occurring during combustion. Observation and morphology analysis of sampled soot via High-Resolution Transmission Electron Microscopy (HR-TEM) are also in progress.</div></div>

The Liquidus Temperature for Methanol‐Water Mixtures at High Pressure and Low Temperature, With Application to Titan

AbstractMethanol is a potentially important impurity in subsurface oceans on Titan and Enceladus. We report measurements of the freezing of methanol‐water samples at pressures up to 350 MPa using a volumetric cell with sapphire windows. For low concentrations of methanol, the liquidus temperature is typically a few degrees below the corresponding ice freezing point, while at high concentrations it follows the pure methanol trend. In the Ice‐III regime, we observe several long‐lived metastable states. The results suggest that methanol is a more effective antifreeze than previously estimated and might have played an important role in the development of Titan's subsurface ocean.

Optical windows as materials for high-speed shock wave detectors

Experimental studies of high-velocity (1-4 km/s) impacts of laser-launched flyer plates with polycrystalline, glassy or polymer windows were performed, with the intent of understanding and assessing the use of optical windows as high-speed solid-state shock wave detector materials. The problem is that the detector material undergoes radical physical transformations during the measurement. Here we present a simplified model where the detector material transformations are described as velocity and time dependent changes in shock impedance. The window materials were used to study the detonation shock produced by nitromethane, which is about 20 GPa and 10 ns. Reference experiments producing shocks in this pressure and duration range characterized how the shock impedances changed with impact velocity and shock duration. Sapphire, CaF2 and LiF windows had the fastest response to the detonation shocks, while the polymer windows had a sluggish response. Pyrex and BK7 were the best of the glassy windows.

Dynamic reflectance changes in high-purity zirconium when it is shocked from the α to ω phase

Flash lamp-illuminated integrating spheres have been used to measure the dynamic reflectance at the interface between a shocked metal target and a window maintaining the shock stress. In conjunction with radiance measurements, this method was recently used to study the pressure versus temperature phase boundary of the beta phase to body-centered-tetragonal transition of tin at around 13 GPa and, in separate experiments, to show a relationship between the reflectance and the phase fraction. We have used this technique to measure the ratio, R, of the dynamic reflectance relative to the ambient value for a high-purity zirconium sample attached to a sapphire window to study the alpha to omega phase transition. Nine experiments cover the range of stress, σ, from 4 to 16 GPa at six wavelengths from 500 to 1550 nm. The two phases in zirconium differ in volume by <1%, so a phase change between them can be difficult to identify from anomalies in the particle velocity measured on the shock Hugoniot. The phase boundary is believed to cross the Hugoniot around 3 GPa, but dynamically it is observed at much higher stresses >6 GPa. Our results show that the relative reflectance decreases upon initial shock in the alpha state but increases as the material transforms to its omega state. The slope dR/dσ changes the sign around the phase transition. For shocks below 6 GPa, dR/dσ < 0, and for σ above 10 GPa, dR/dσ > 0. In the stress region between 6 and 10 GPa, dR/dσ varies somewhat, perhaps due to the band structure or because the transition is incomplete there.

Selective Reflection of Laser Radiation from Ultrathin Layers of Cesium Atomic Vapors Confined in a Nanocell

The effect of the van der Waals interaction of cesium atoms with the sapphire windows of a nanocell was experimentally investigated using the selective reflection process. The distance L between the windows varied in the range of 50–2000 nm and the nanocell was filled with the vapors of cesium atoms. For the Cs atoms (the transition 6S1/2 → 6P1/2), the C3 coefficient of the van der Waals interaction with the sapphire windows of the nanocell is measured. It is shown that it is possible to determine the magnetic fields with the spatial resolution of 70 nm using the selective reflection spectrum and, consequently, both the homogeneous and highly gradient magnetic fields can be measured.

High pressure phase equilibrium data for carbon dioxide, methyl methacrylate and poly (dimethylsiloxane) systems

This paper investigates high-pressure phase transitions for the binary system carbon dioxide (CO2) + methyl methacrylate (MMA) and for the ternary system CO2 + MMA + poly (dimethylsiloxane) vinyl terminated (PDMS-V). The experiments were carried out using the static-synthetic method in a stainless steel equilibrium cell with a variable-volume, including piston and sapphire window, at temperatures of 323.15, 333.15, 343.15 and 353.15 K and the molar fraction ranging from 0.6949 to 0.9499 and 0.6833 to 0.9444 for the binary and ternary systems, respectively. For the binary system, phase transition was determined from the liquid region to the two-phase region. High miscibility of carbon dioxide in MMA was observed with a significant volumetric expansion of the liquid phase. The surfactant PDMS-V was added to this binary system in order to investigate its effect on the phase behavior. For the ternary system CO2 + MMA + PDMS-V, phase transitions were observed from the liquid homogeneous phase until the two-phase region. The results indicate that the addition of PDMS-V led to a small increase in the phase transition pressure, and for the liquid-liquid region a large increase in the phase transition pressure of the system occurred at all temperatures.

Development of a tunable diode laser sensor for CO concentration analysis at laboratory-scale conditions for in situ combustion tests of heavy crude oils.

A tunable diode laser-based sensor is reported to monitor carbon monoxide (CO) concentration under conditions similar to those of laboratory-scale tests used to characterize the behavior of heavy crude oil during in situ combustion (ISC). The sensor uses a DFB diode laser operating over the spectral range of the rotational transition R(11) of the first overtone, wherein simulations of spectral absorption bands for CO, CO2, and H2O showed minimal spectral interference. The absorption spectra were calculated using the HiTran 2008 database at temperatures varying between 150°C and 800°C, pressures from 1 to 5atm, and the typical concentration of major species in ISC characterization experiments. The measurements of CO concentration were conducted at ambient temperature and pressure in a static glass cell of borosilicate, with a path length of 3.81cm, to validate the CO sensor architecture under controlled laboratory environments. The calibration curve for CO obtained by quantifying the optical density at the line center of R(11) for a molar-concentration range between 0.7% and 3.4% demonstrated a linear response (coefficient of determination of 0.9986). Experiments at 4atm and 600K were carried out in a custom-designed optical chamber with two optical wedged sapphire windows (2°) to avoid the etalon effect. CO-absorption spectra were validated by a comparative study with the HiTran database, while a calibration-free methodology using scanned-wavelength direct absorption was investigated for future characterizing experiments involving ISC. Signal to noise ratios (SNRs) were above 40 in the optical chamber and higher than 14 in the glass cell. The TDL sensor was also successfully validated during real ISC experiments involving Colombian heavy crude oil. The calibration and oxidation experiments showed the potential of TDL-based sensors in the region of 2.3μm for non-invasive, real-time, and in situ measurements of carbon monoxide generated at similar conditions to those of lab-scale experimental ISC tests.

DyeLIF™: A New Direct‐Push Laser‐Induced Fluorescence Sensor System for Chlorinated Solvent DNAPL and Other Non‐Naturally Fluorescing NAPLs

AbstractDyeLIF™ is a new version of laser‐induced fluorescence (LIF) for high‐resolution three‐dimensional subsurface mapping of nonaqueous phase liquids (NAPLs) in the subsurface. DyeLIF eliminates the requirement that the NAPL contains native fluorophores (such as those that occur in compounds like polynuclear aromatic hydrocarbons [PAHs]) and can therefore be used to detect chlorinated solvents and other nonfluorescing NAPLs that had previously been undetectable with conventional LIF tools. With DyeLIF, an aqueous solution of water and nontoxic hydrophobic dye is continuously injected ahead of the sapphire detection window while the LIF probe is being advanced in the subsurface. If soil containing NAPL is penetrated, the injected dye solvates into the NAPL within a few milliseconds, creating strong fluorescence that is transmitted via fiber‐optic filaments to aboveground optical sensors. A detailed field evaluation of the novel DyeLIF technology was performed at a contaminated industrial site in Lowell, Massachusetts, USA where chlorinated solvent dense nonaqueous phase liquid (DNAPL) persists below the water table in sandy sediments. Continuously cored boreholes were drilled adjacent to 5 of 30 DyeLIF probes that were advanced at that site. The cores were subsampled in high resolution to generate discrete‐depth soil samples as splits at the same depths where DNAPL was detected in the colocated DyeLIF probes. The cores were analyzed above ground using (1) colorimetric screening using hydrophobic dye tests, (2) laboratory extraction and quantitative chemical analysis, (3) “Benchtop” DyeLIF, and (4) volumetric moisture content. Correlation between DyeLIF and aboveground analyses of the soil cores was excellent: 98% agreement with positive DNAPL detections in samples where DNAPL pore saturations were >0.7% (based on quantitative soil analyses) and the ex situ tests. DyeLIF produced the equivalent of one aboveground colorimetric dye test every 0.2 inch (0.5 cm) of probing. With average daily probing of 395 linear feet (120.4 m), this was the equivalent of 12,039 discrete‐depth colorimetric dye tests/day. Because DyeLIF is an in situ measurement, there are no issues with soil core recovery like there would be for conventional ex situ colorimetric dye tests and 100% characterization of the probed intervals is achieved. Tracking the injection rate and pressure of the dye solution provides simultaneous data regarding relative soil permeability, similar to other direct push (DP) hydraulic profiling tools. Conventional LIF is considered the premier DP tool to identify and map NAPL containing PAHs in the subsurface or confirm its absence. While chlorinated solvent DNAPLs at some field sites contain impurities (e.g., solvated greases or oils) that make them detectable with conventional LIF techniques, at other sites, the DNAPL cannot be detected with conventional LIF. At such sites, the injection of a hydrophobic dye ahead of the sapphire window with the DyeLIF system now makes the LIF technology applicable to the many types of NAPLs that were previously invisible using conventional LIF techniques.

Optical shaping of surface metal microstructures via nondiffracting beam controlled atomic deposition

The first experimental realization of the non-diffracting Bessel beam technique for micro-structuring of thin rubidium metallic films on the sapphire surface is reported. Rubidium atoms were deposited onto the cool sapphire windows from the heated central region of the evacuated cell under simultaneous illumination by a Bessel beam at 532 nm wavelength and 4.5 W/cm2 intensity. The approach of the optically controlled atomic deposition is based on the strong non-thermal photo-desorption of atoms from illuminated areas of dielectric surface diminishing the surface density of adsorbed atoms below the threshold of nucleation process, while in the dark areas concentration of adsorbed atoms exceeds the critical value and a metal film starts to grow. As a result, the annular Bessel beam optical pattern with 40 μm periodicity was reproduced with high contrast in the Rb deposits, thus creating the annularly micro-structured metal film on the sapphire surface. The diffraction efficiency of the metal grating with the estimated thickness of ∼40 nm was measured to be about 1.8%.

Evaluation and application of the optical image profiler (OIP) a direct push probe for photo-logging UV-induced fluorescence of petroleum hydrocarbons

The presence of free phase petroleum fuels in the subsurface (often called light nonaqueous phase liquids/LNAPL) is a hazard in almost every town and city in the modern world. Leaking underground storage tanks and the resulting contamination and hazards have proven to be a challenge to investigate and remediate. One issue is adequately characterizing the presence and spatial extent of LNAPLs in the subsurface. Experience has shown that conventional soil coring methods and groundwater monitoring methods are fraught with limitations that can lead to significant errors in the estimation of the amount and spatial distribution of LNAPLs in the subsurface. This leads to the development of inaccurate conceptual site models and costly errors in remedial actions. A new direct push logging tool, the optical image profiler (OIP), has been developed to obtain high resolution site characterization data to more accurately define the presence and extent of LNAPLs in unconsolidated materials. The OIP system uses a downhole ultraviolet light-emitting diode to induce fluorescence of fuel LNAPL. A small complimentary metal–oxide–semiconductor camera mounted inside the probe behind a sapphire window captures photographic images of visible range fluorescence as the probe is advanced by direct push methods. In situ images of subsurface fuel fluorescence have not previously been available to the investigator and may further the understanding of LNAPL behavior. The OIP software also provides a log of percent area fluorescence (%AF) based on analysis of the images. An electrical conductivity (EC) dipole on the probe provides a log of bulk formation EC that is often a good indicator of formation lithology. The information presented here explains the basic design and operation of the OIP system in the field. Bench tests confirm the capability of the OIP system to detect a range of petroleum fuels. Field studies with the tandem EC and %AF logs are used to identify LNAPL and its migration pathways in the subsurface. These capabilities can improve the management and remediation of LNAPL-impacted sites and reduce long-term costs associated with cleanup and closure.

High efficiency Dual-Cycle Conversion System using Kr-85

This paper discusses the use of one of the safest isotopes known isotopes, Kr-85, as a candidate fuel source for deep space missions. This isotope comes from 0.286% of fission events. There is a vast quantity of Kr-85 stored in spent fuel and it is continually being produced by nuclear reactors. In using Kr-85 with a novel Dual Cycle Conversion System (DCCS) it is feasible to boost the system efficiency from 26% to 45% over a single cycle device while only increasing the system mass by less than 1%. The Kr-85 isotope is the ideal fuel for a Photon Intermediate Direct Energy Conversion (PIDEC) system. PIDEC is an excellent choice for the top cycle in a DCCS. In the top cycle, ionization and excitation of the Kr-85:Cl gas mixture (99% Kr and 1% Cl) from beta particles creates KrCl* excimer photons which are efficiently absorbed by diamond photovoltaic cells on the walls of the pressure vessels. The benefit of using the DCCS is that Kr-85 is capable of operating at high temperatures in the primary cycle and the residual heat can then be converted into electrical power in the bottom cycle which uses a Stirling Engine. The design of the DCCS begins with a spherical pressure vessel of radius 13.7 cm with 3.7 cm thick walls and is filled with a Kr-85:Cl gas mixture. The inner wall has diamond photovoltaic cells attached to it and there is a sapphire window between the diamond photovoltaic cells and the Kr-85:Cl gas mixture which shields the photovoltaic cells from beta particles. The DCCS without a gamma ray shield has specific power of 6.49 W/kg. A removable 6 cm thick tungsten shield is used to safely limit the radiation exposure levels of personnel. A shadow shield remains in the payload to protect the radiation sensitive components in the flight package. The estimated specific power of the unoptimized system design in this paper is about 2.33 W/kg. The specific power of an optimized system should be higher. The Kr-85 isotope is relatively safe because it will disperse quickly in case of an accident and if it enters the lungs there is no significant biological half-life.

Effect of acoustic impedance matching on kinetics of titanium phase transformation

The phase transition experiments under ramp wave compression of titanium have been done by using a magnetic diven device CQ-4, and the influence of the acoustic impedance of the back surface of titanium on the phase transition has been studied. The experimental results show that when the acoustic impedance of the window is low, free surface or LiF, the particle velocity corresponding to the beginning of phase transition is about 408.9 m/s, while at the high impedance sapphire window, is about 373.9 m/s. The pressures corresponding to the characteristic velocities are not the phase change onset pressures. A simulation was done to well describe this complicated dynamic response including physical models of multi-phase equation of state based on Helmholtz free energy, strength model, and non-equilibrium dynamic equation of phase transition. The calculated results are in excellent agreement with the experimental data, and they exhibit the dynamic physical characteristics of Tin involving the elastoplastic transition and evolution of mass fraction of different phase. The results show that the velocity wave forms of the samples near the loading surface are the same, but the amplitude of the wave forms varies greatly due to the impedance matching of Tin and windows in the vicinity of Tin’s rear surface. The phase transition pressure of Ti is about 10.5 GPa, which is a rate dependent non-equilibrium dynamic process. In the pressure-volume thermodynamic plane, the calculated isentrope coincides with Hugoniot before phase transition, but is below the Hugoniot after phase change. The obvious decrease in sound velocity after phase transition is due to the discontinuity of the specific volume due to phase transition.

Frequency-agile gyrotron for electron decoupling and pulsed dynamic nuclear polarization

We describe a frequency-agile gyrotron which can generate frequency-chirped microwave pulses. An arbitrary waveform generator (AWG) within the NMR spectrometer controls the microwave frequency, enabling synchronized pulsed control of both electron and nuclear spins. We demonstrate that the acceleration of emitted electrons, and thus the microwave frequency, can be quickly changed by varying the anode voltage. This strategy results in much faster frequency response than can be achieved by changing the potential of the electron emitter, and does not require a custom triode electron gun. The gyrotron frequency can be swept with a rate of 20 MHz/μs over a 670 MHz bandwidth in a static magnetic field. We have already implemented time-domain electron decoupling with dynamic nuclear polarization (DNP) magic angle spinning (MAS) with this device. In this contribution, we show frequency-swept DNP enhancement profiles recorded without changing the NMR magnet or probe. The profile of endofullerenes exhibits a DNP profile with a <10 MHz linewidth, indicating that the device also has sufficient frequency stability, and therefore phase stability, to implement pulsed DNP mechanisms such as the frequency-swept solid effect. We describe schematics of the mechanical and vacuum construction of the device which includes a novel flanged sapphire window assembly. Finally, we discuss how commercially available continuous-wave gyrotrons can potentially be converted into similar frequency-agile high-power microwave sources.

An electrochemical cell with sapphire windows for operando synchrotron X-ray powder diffraction and spectroscopy studies of high-power and high-voltage electrodes for metal-ion batteries.

A new multi-purpose operando electrochemical cell was designed, constructed and tested on the Swiss-Norwegian Beamlines BM01 and BM31 at the European Synchrotron Radiation Facility. Single-crystal sapphire X-ray windows provide a good signal-to-noise ratio, excellent electrochemical contact because of the constant pressure between the electrodes, and perfect electrochemical stability at high potentials due to the inert and non-conductive nature of sapphire. Examination of the phase transformations in the Li1-xFe0.5Mn0.5PO4 positive electrode (cathode) material at C/2 and 10C charge and discharge rates, and a study of the valence state of the Ni cations in the Li1-xNi0.5Mn1.5O4 cathode material for Li-ion batteries, revealed the applicability of this novel cell design to diffraction and spectroscopic investigations of high-power/high-voltage electrodes for metal-ion batteries.

Mars analog minerals’ spectral reflectance characteristics under Martian surface conditions

We investigated the spectral reflectance properties of minerals under a simulated Martian environment. Twenty-eight different hydrated or hydroxylated phases of carbonates, sulfates, and silica minerals were selected based on past detection on Mars through spectral remote sensing data. Samples were ground and dry sieved to <45 µm grain size and characterized by XRD before and after 133 days inside a simulated Martian surface environment (pressure 5 Torr and CO2 fed). Reflectance spectra from 0.35 to 4 µm were taken periodically through a sapphire (0.35–2.5 µm) and zinc selenide (2.5–4 µm) window over a 133-day period. Mineral stability on the Martian surface was assessed through changes in spectral characteristics. Results indicate that the hydrated carbonates studied would be stable on the surface of Mars, only losing adsorbed H2O while maintaining their diagnostic spectral features. Sulfates were less stable, often with shifts in the band position of the SO, Fe, and OH absorption features. Silicas displayed spectral shifts related to SiOH and hydration state of the mineral surface, while diagnostic bands for quartz were stable. Previous detection of carbonate minerals based on 2.3–2.5 µm and 3.4–3.9 µm features appears to be consistent with our results. Sulfate mineral detection is more questionable since there can be shifts in band position related to SO4. The loss of the 0.43 µm Fe3+ band in many of the sulfates indicate that there are fewer potential candidates for Fe3+ sulfates to permanently exist on the Martian surface based on this band. The gypsum sample changed phase to basanite during desiccation as demonstrated by both reflectance and XRD. Silica on Mars has been detected using band depth ratio at 1.91 and 1.96 µm and band minimum position of the 1.4 µm feature, and the properties are also used to determine their age. This technique continues to be useful for positive silica identifications, however, silica age appears to be less consistent with our laboratory data. These results will be useful in spectral libraries for characterizing Martian remote sensed data.

Spectrometer-based refractive index and dispersion measurement using low-coherence interferometry with confocal scanning.

This paper describes a technique for measuring refractive index and thickness of transparent plates using a fibre-optic low-coherence interferometer. The interferometer is used to independently measure quantities related to the phase and group refractive indices, np and ng, of the material under investigation. Additionally, the dispersion of the phase index dependent quantity is measured by taking advantage of the range of wavelengths available from a broadband source. These three quantities are related to simultaneously yield np and ng as well as the geometrical thickness t of the sample. Measurements are presented for a range of transparent materials including measurements of the ordinary and extraordinary refractive indices of a birefringent sapphire window. The mean percentage errors across all the samples tested were 0.09% for np, 0.08% for np, and 0.11% for t.

Broad-band anti-reflective pore-like sub-wavelength surface nanostructures on sapphire for optical windows

Compared with conventional anti-reflective film, an anti-reflective sub-wavelength surface structure provides an ideal choice for a sapphire optical window especially in harsh environments. However, it is still a challenge to obtain a sapphire anti-reflective surface microstructure because of its high hardness and chemical inertness. In this paper, combined with optical simulation, we proposed a facile method based on the anodic oxidation of aluminum film and following epitaxial annealing. Al thin film was deposited on a sapphire substrate by magnetron sputtering, and anodic oxidation was then performed to prepare surface pore-like structures on the Al film. Followed by two-step annealing, both the anodic oxidized coating and underlying unoxidized Al film were transformed totally into alumina. The parameters of anodic oxidation were analyzed to obtain the optimal pore-like structures for the antireflection in the mid-infrared and visible spectrum regions, respectively. Finally, the optimized surface sub-wavelength nanostructure on sapphire can increase the transmittance by 7% in the wavelength range of 3000–5000 nm and can increase 13.2% significantly for visible spectrum region, respectively. Meanwhile, the surface wettability can be also manipulated effectively. The preparation of surface pore-like sub-wavelength structure by the annealing of anodic oxidized aluminum film on sapphire is a feasible, economical and convenient approach and can find the applications for various optoelectronic fields.

Phase transformation kinetics of zirconium under ramp wave loading with different windows

The effect of window acoustic impedance on the wave profile of phase transition of zirconium under ramp wave compression is investigated in experiment and simulation. In the experiments, a ramp wave driven by magnetic pressure is applied to the zirconium samples backed windows with different acoustic impedances such as LiF, sapphire and free surface based on the compact pulsed power generator CQ-4. The experimental wave profiles measured by an advanced laser interference velocimeter show that the characteristic particle velocity of the onset phase transition from to is about 331.0 m/s in the conditions of LiF widow and free surface with low acoustic impedance, and it is approximately 301.9 m/s for the sapphire window with higher acoustic impedance. The corresponding onset pressure of phase transition varies from about 9.14 GPa to 8.27 GPa. The result shows that this onset pressure of phase transition, which is affected by diverse factors, is not the inherent value of phase transition belonging to the material properties. In order to describe these dynamic responses in experiment well, the numerical simulation of phase transition dynamics of zirconium is conducted in one-dimensional hydrodynamic code, in which included are the muti-phase equation of state based on Helmholtz free energy, the equation of non-equilibrium phase transition dynamics, and Steinberg constitutive relationship. The simulated results show that they can reflect the physical processes of elasto-plastic transition and - phase transition as well, which are excellently consistent with the experimental data. The relaxation times of - phase transition in three different acoustic impedance experiments are nearly the same (30 ns), and their finishing times of phase transition are all about 100 ns. The calculated quasi-isentrope of zirconium below 20 GPa in the pressure-volume and temperature-pressure thermodynamic planes shows that the isentrope and shock adiabat exhibit tiny difference before phase transition, and then separate gradually with the increase of pressure. The isentrope lies below the shock adiabat after the onset of phase transition. At about 20 GPa, the temperature of zirconium under ramp wave loading is bout 100 K lower than that under shock loading. Meanwhile, the abrupt change of volume at phase transition causes the Lagrange sound speed to reduce about 7% and then comes back to the bulk sound speed again after the phase transition has been finished.