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At least 217 records · Page 12

Preparation and stress evolution of sol–gel SiO{sub 2} antireflective coatings for small-size anisotropic lithium triborate crystals

Lithium triborate (LiB{sub 3}O{sub 5}, LBO) crystal is now one of the most useful nonlinear optical materials for frequency conversion of high power lasers. The use of the crystal, however, has been hampered by the unavailability of antireflective (AR) coatings with high laser damage resistance. In this work, a “point contact” dip-coating method is developed to prepare sol–gel SiO{sub 2} AR coatings on small-size LBO crystals. Using this approach, we obtain a homogenous coating surface on an 8 mm×8 mm×3 mm LBO crystal. The stress measurements show that the stresses in sol–gel SiO{sub 2} coatings vary with the time of natural drying, which is beyond our expectation. The anisotropic Young’s modulus of the LBO crystal and the different evolution tendency of the stress in the different SiO{sub 2} coating layers are found to be responsible for the crack of the double-layer AR coatings on anisotropic LBO crystal. Meanwhile, the resulting coatings on LBO crystal achieve a LIDT of over 15 J/cm{sup 2} (532 nm, 3ns) and the coated LBO is expected to have a transmittance of over 99% at 800 nm.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Application of fiber bridging models to fatigue crack growth in unidirectional titanium matrix composites

Several fiber bridging models were reviewed and applied to study the matrix fatigue crack growth behavior in center notched (0)(sub 8) SCS-6/Ti-15-3 and (0)(sub 4) SCS-6/Ti-6Al-4V laminates. Observations revealed that fatigue damage consisted primarily of matrix cracks and fiber matrix interfacial failure in the (0)(sub 8) SCS-6/Ti-15-3 laminates. Fiber-matrix interface failure included fracture of the brittle reaction zone and cracking between the two carbon rich fiber coatings. Intact fibers in the wake of the matrix cracks reduce the stress intensity factor range. Thus, an applied stress intensity factor range is inappropriate to characterize matrix crack growth behavior. Fiber bridging models were used to determine the matrix stress intensity factor range in titanium metal matrix composites. In these models, the fibers in the wake of the crack are idealized as a closure pressure. An unknown constant frictional shear stress is assumed to act along the debond or slip length of the bridging fibers. The frictional shear stress was used as a curve fitting parameter to available data (crack growth data, crack opening displacement data, and debond length data). Large variations in the frictional shear stress required to fit the experimental data indicate that the fiber bridging models in their present form lack predictive capabilities. However, these models provide an efficient and relatively simple engineering method for conducting parametric studies of the matrix growth behavior based on constituent properties.

Bakuckas, J. G., Jr.↗

Effects of UV Aging on the Cracking of Titanium Oxide Layer on Poly(ethylene terephthalate) Substrate: Preprint

Thin oxide and metal films deposited on polymer substrates is an emerging technology for advanced reflectors for concentrated solar power applications, due to their unique combination of light weight, flexibility and inexpensive manufacture. Thus far, there is little knowledge on the mechanical integrity or structural persistence of such multi-layer thin film systems under long-term environmental aging. In this paper, the cracking of a brittle titanium dioxide layer deposited onto elasto-plastic poly(ethylene terephthalate) (PET) substrate is studied through a combination of experiment and modeling. In-situ fragmentation tests have been conducted to monitor the onset and evolution of cracks both on pristine and on samples aged with ultraviolet (UV) light. An analytical model is presented to simulate the cracking behavior and to predict the effects of UV aging. Based on preliminary experimental observation, the effect of aging is divided into three aspects and analyzed independently: mechanical property degradation of the polymer substrate; degradation of the interlayer between substrate and oxide coating; and internal stress-induced cracks on the oxide coating.

14 SOLAR ENERGY↗

Burst and oxidation behavior of Cr-coated Zirlo during simulated LOCA testing

We report Cr-coated Zr-alloys are a near-term cladding concept to improve reactor safety during accident scenarios. Burst and steam oxidation behavior of bare and Cr-coated Zirlo claddings were examined under simulated loss-of-coolant accident conditions. The 4.4 µm coating had no substantial effect on ballooning or opening geometry but did increase burst temperatures at higher pressures. The coating reduced steam oxidation of the cladding compared to bare specimens, but in regions of high strain, the coating developed through-cracks allowing rapid underlying zirconia formation.

36 MATERIALS SCIENCE↗

Environmental testing of REI-Mullite thermal protection system for the space shuttle orbiter

Tests conducted to evaluate performances in the natural environments of salt spray, humidity, rain, vacuum, and cryogenic temperatures have shown the ceramic mullite fiber is completely compatible and that these environments have no adverse effects on subsequent mission performance. Rain erosion testing has indicated a damage threshold that must be accounted for in the final design. Tests conducted to evaluate the performance of ceramic mullite fiber to induced acoustic, re-entry, and structural load environments again have shown complete capability to fulfill mission environments. Although minor cracking of the sidewall coating was seen to occur throughout the induced environment test program, sidewall designs configured to provide increased flexibility have been successfully tested.

Gluck, R.↗

Oxidation and protection of fiberglass-epoxy composite masts for photovoltaic arrays in the low Earth orbital environment

Fiberglass-epoxy composites are considered for use as structural members for the mast of the space station solar array panel. The low Earth orbital environment in which space station is to operate is composed mainly of atomic oxygen, which has been shown to cause erosion of many organic materials and some metals. Ground based testing in a plasma asher was performed to determine the extent of degradation of fiberglass-epoxy composites when exposed to a simulated atomic oxygen environment. During exposure, the epoxy at the surface of the composite was oxidized, exposing individual glass fibers which could easily be removed. Several methods of protecting the composite were evaluated in an atomic oxygen environment and with thermal cycling and flexing. The protection techniques evaluated to date include an aluminum braid covering, an indium-tin eutectic and a silicone based paint. The open aluminum braid offered little protection while the CV-1144 coating offered some initial protection against atomic oxygen, but appears to develop cracks which accelerate degradation when flexed. Coatings such as the In-Sn eutectic may provide adequate protection by containing the glass fibers even though mass loss still occurs.

Rutledge, Sharon K.↗

Prediction Of Critical Crack Sizes In Solar Cells

Report presents theoretical analysis of cracking in Si and GaAs solar photovoltaic cells subjected to bending or twisting. Analysis also extended to predict critical sizes for cracks in Ge substrate coated with thin film of GaAs. Analysis leads to general conclusions. Approach and results of study useful in development of guidelines for acceptance or rejection of slightly flawed cells during manufacture.

Chen, Chern P.↗

Effects of Interface Coating and Nitride Enhancing Additive on Properties of Hi-Nicalon SiC Fiber Reinforced Reaction-Bonded Silicon Nitride Composites

Strong and tough Hi-Nicalon SiC fiber reinforced reaction-bonded silicon nitride matrix composites (SiC/ RBSN) have been fabricated by the fiber lay-up approach. Commercially available uncoated and PBN, PBN/Si-rich PBN, and BN/SiC coated SiC Hi-Nicalon fiber tows were used as reinforcement. The composites contained approximately 24 vol % of aligned 14 micron diameter SiC fibers in a porous RBSN matrix. Both one- and two-dimensional composites were characterized. The effects of interface coating composition, and the nitridation enhancing additive, NiO, on the room temperature physical, tensile, and interfacial shear strength properties of SiC/RBSN matrix composites were evaluated. Results indicate that for all three coated fibers, the thickness of the coatings decreased from the outer periphery to the interior of the tows, and that from 10 to 30 percent of the fibers were not covered with the interface coating. In the uncoated regions, chemical reaction between the NiO additive and the SiC fiber occurs causing degradation of tensile properties of the composites. Among the three interface coating combinations investigated, the BN/SiC coated Hi-Nicalon SiC fiber reinforced RBSN matrix composite showed the least amount of uncoated regions and reasonably uniform interface coating thickness. The matrix cracking stress in SiC/RBSN composites was predicted using a fracture mechanics based crack bridging model.

Bhatt, Ramakrishana T.↗

Interaction Studies of Ceramic Vacuum Plasma Spraying for the Melting Crucible Materials

Candidate coating materials for re-usable metallic nuclear fuel crucibles, TaC, TiC, ZrC, ZrO2, and Y2O3, were plasmasprayed onto a niobium substrate. The microstructure of the plasma-sprayed coatings and thermal cycling behavior were characterized, and U-Zr melt interaction studies were carried out. The TaC and Y2O3 coating layers had a uniform thickness, and high density with only a few small closed pores showing good consolidation, while the ZrC, TiC, and ZrO2 coatings were not well consolidated with a considerable amount of porosity. Thermal cycling tests showed that the adhesion of the TiC, ZrC, and ZrO2 coating layers with niobium was relatively weak compared to the TaC and Y2O3 coatings. The TaC and Y2O3 coatings had better cycling characteristics with no interconnected cracks. In the interaction studies, ZrC and ZrO2 coated rods showed significant degradations after exposure to U-10 wt.% Zr melt at 1600 degrees C for 15 min., but TaC, TiC, and Y2O3 coatings showed good compatibility with U-Zr melt.

99 GENERAL AND MISCELLANEOUS↗

Effects of high temperature treatment on microstructure and mechanical properties of laser-clad NiCrBSi/WC coatings on titanium alloy substrate

Laser-clad composite coatings on the Ti6Al4V substrate were heat-treated at 700, 800, and 900 °C for 1 h. The effects of post-heat treatment on the microstructure, microhardness, and fracture toughness of the coatings were investigated by scanning electron microscopy, X-ray diffractometry, energy dispersive spectroscopy, and optical microscopy. The wear resistance of the coatings was evaluated under dry reciprocating sliding friction at room temperature. The coatings mainly comprised some coarse gray blocky (W,Ti)C particles accompanied by the fine white WC particles, a large number of black TiC cellular/dendrites, and the matrix composed of NiTi and Ni{sub 3}Ti; some unknown rich Ni- and Ti-rich particles with sizes ranging from 10 nm to 50 nm were precipitated and uniformly distributed in the Ni{sub 3}Ti phase to form a thin granular layer after heat treatment at 700 °C. The granular layer spread from the edge toward the center of the Ni{sub 3}Ti phase with increasing temperature. A large number of fine equiaxed Cr{sub 23}C{sub 6} particles with 0.2–0.5 μm sizes were observed around the edges of the NiTi supersaturated solid solution when the temperature was further increased to 900 °C. The microhardness and fracture toughness of the coatings were improved with increased temperature due to the dispersion-strengthening effect of the precipitates. Dominant wear mechanisms for all the coatings included abrasive and delamination wear. The post-heat treatment not only reduced wear volume and friction coefficient, but also decreased cracking susceptibility during sliding friction. Comparatively speaking, the heat-treated coating at 900 °C presented the most excellent wear resistance. - Highlights: • TiC + WC reinforced intermetallic compound matrix composite coatings were produced. • The formation mechanism of the reinforcements was analyzed. • Two precipitates were generated at elevated temperature. • Cracking susceptibility and microhardness of the coatings were improved. • Post-heat treatment enhances wear resistance of the coatings.

36 MATERIALS SCIENCE↗

Laser damage of crazed electron-beam high-reflectors following infrared and ultraviolet irradiation in the nanosecond pulse regime

Laser damage of optical components can be a limiting factor in scaling the energetics of high-peak and average power laser systems. Specifically for optical coatings, damage under nanosecond pulsed irradiation is initiated by pre-existing defects in the coating layers, including those that cause discontinuities in the structure, like craze lines. Crazing or cracking in a multilayer dielectric optical coating is induced when the overall coating stress is sufficiently tensile, and is an occasionally observed issue when employing more porous deposition techniques like electron-beam evaporation. Here, in this study, electron-beam high-reflectors were fabricated utilizing process parameters that are known to induce crazing based on prior processing history to systematically evaluate the impact of crazing on reflector damage performance for 1064 and 355 nm lasers. The crazing that was observed was apparently nucleated at nodular defects. When the cross-section of these nodules was investigated, it was observed that there were cracks into the fused silica substrate of approximately 5 µm in depth. The craze lines were irradiated with 1064 and 355 nm light at fluences slightly above the onset of damage initiation fluence of the coating. The 1064 nm irradiated sub-apertures exhibit laser damage but with no spatial correlation with the craze line, whereas the 355 nm irradiated area exhibited many damage sites along the craze line. Finite-difference time-domain electric-field simulations were conducted, and ∼2× field amplification in hafnia was observed for the 355 nm wavelength case. The laser damage can be attributed to a slight electric-field intensification coincidental with an area where UV damage-prone precursors are known to occur. The 355 nm laser damage in uncoated fused silica substrates has been previously correlated to initiate through localized UV absorption at the broken silica bonds in the tips of fractures.

Harthcock, Colin [Lawrence Livermore National Labo↗

Consequences of Atomic Oxygen Interaction With Silicone and Silicone Contamination on Surfaces in Low Earth Orbit

The exposure of silicones to atomic oxygen in low Earth orbit causes oxidation of the surface, resulting in conversion of silicone to silica. This chemical conversion increases the elastic modulus of the surface and initiates the development of a tensile strain. Ultimately, with sufficient exposure, tensile strain leads to cracking of the surface enabling the underlying unexposed silicone to be converted to silica resulting in additional depth and extent of cracking. The use of silicone coatings for the protection of materials from atomic oxygen attack is limited because of the eventual exposure of underlying unprotected polymeric material due to deep tensile stress cracking of the oxidized silicone. The use of moderate to high volatility silicones in low Earth orbit has resulted in a silicone contamination arrival at surfaces which are simultaneously being bombarded with atomic oxygen, thus leading to conversion of the silicone contaminant to silica. As a result of these processes, a gradual accumulation of contamination occurs leading to deposits which at times have been up to several microns thick (as in the case of a Mir solar array after 10 years in space). The contamination species typically consist of silicon, oxygen and carbon. which in the synergistic environment of atomic oxygen and UV radiation leads to increased solar absorptance and reduced solar transmittance. A comparison of the results of atomic oxygen interaction with silicones and silicone contamination will be presented based on the LDEF, EOIM-111, Offeq-3 spacecraft and Mir solar array in-space results. The design of a contamination pin-hole camera space experiment which uses atomic oxygen to produce an image of the sources of silicone contamination will also be presented.

Banks, Bruce A.↗

Deformation mechanisms in amorphous Ni–Mo–P films coated on CoCrFeNi high-entropy alloys

The Ni–Mo–P amorphous films were successfully deposited on the CoCrFeNi high-entropy alloys by electroless plating. This work will focus on reviewing and discussing the ambient-temperature mechanical properties, plastic deformation, and cracking mode of the coating-substrate system. The yielding strength (σ y ) and ultimate tensile strength (UTS) of the specimen plating for 1 h were 260 and 760 MPa, respectively, with 44.4% (σ y ) and 14.2% (UTS) improvement contrast to the uncoated HEAs (σ y and UTS are 180 MPa and 560 MPa, respectively). It is attributed to the back stress and repulsive image stress to suppress the nucleation and mobility of dislocations. Due to the substrate confinement, the deformation model was gradually changed from cracking (with homogeneous flow) to shear banding (with homogeneous flow). Eventually, fully-homogeneous flows occur with reducing the film thickness, and the deformation mechanism map is developed to expound the transition of the deformation mode. The brittle fracture with a high velocity originating from amorphous films leads to cleavage cracking on the surface of the HEA substrate. The thicker film has higher crack velocity and causes deeper cracks penetration into the substrate, reducing the substrate ductility.

36 MATERIALS SCIENCE↗

Atomic oxygen interactions with protected organic materials on the Long Duration Exposure Facility (LDEF)

The Long Duration Exposure Facility (LDEF) has provided an excellent opportunity to understand the nature of directed atomic oxygen interactions with protected polymers and composites. Although there were relatively few samples of materials with protective coatings on their external surfaces on LDEF which were exposed to a high atomic oxygen fluence, analysis of such samples has enabled an examination of the shape of atomic oxygen undercut cavities at defect sites in the protective coatings. Samples of front-surface aluminized (Kapton) polyimide were inspected by scanning electron microscopy to identify and measure crack defects in the aluminum protective coatings. After chemical removal of the aluminum coating, measurements were also made of the width of the oxidized undercut cavities below the crack defects. The LDEF flight undercut cavity geometries were then compared with Monte Carlo computational model undercut cavity predictions. The comparison of the LDEF results and computational modeling indicates agreement in specific undercut cavity geometries for atomic oxygen reaction probabilities dependent upon the 0.68 to 3.0 power of the energy. However, no single energy dependency was adequate to replicate flight results over a variety of aluminum crack widths.

Banks, Bruce A.↗

Thermal and stress analysis of thermal barrier coatings

An analysis has been performed that predicts the thermomechanical behavior of thermal barrier coated specimens. The analysis predicts the behavior during both plasma spray coating application and burner rig testing conditions simulating engine operation. The analysis was accomplished through utilization of one-dimensional through thickness and two-dimensional finite element calculations. The results of these calculations showed that specimens with a substrate control temperature between 300 F and 600 F would be optimum. Controlling substrate temperature was found to have a more dominant effect on the mechanical strains than the ceramic or substrate thicknesses. The predicted stresses and mechanical strains at the bond-coating interface are large enough to cause cracks in this region where post-test observations have determined coating failures originate.

Cassenti, B. N.↗

Operando study of mechanical integrity of high-volume expansion Li-ion battery anode materials coated by Al 2 O 3

Group IV elements and their oxides, such as Si, Ge, Sn and SiO have much higher theoretical capacity than commercial graphite anode. However, these materials undergo large volume change during cycling, resulting in severe structural degradation and capacity fading. Al 2 O 3 coating is considered an approach to improve the mechanical stability of high-capacity anode materials. To understand the effect of Al 2 O 3 coating directly, we monitored the morphology change of coated/uncoated Sn particles during cycling using operando focused ion beam–scanning electron microscopy. Here, the results indicate that the Al 2 O 3 coating provides local protection and reduces crack formation at the early stage of volume expansion. The 3 nm Al 2 O 3 coating layer provides better protection than the 10 and 30 nm coating layer. Nevertheless, the Al 2 O 3 coating is unable to prevent the pulverization at the later stage of cycling because of large volume expansion.

25 ENERGY STORAGE↗

Radiation-Resistant Ti/BN Coatings: Insights From 171 Days Exposure to Space Radiation and Atomic Oxygen in Low Orbit

Atmospheric Plasma Spray (APS) and Vacuum Plasma Spray (VPS) techniques were used to develop Ti/2 vol.% hBN coatings, for extreme space environments and tested aboard the International Space Station as part of the MISSE-17 (Materials International Space Station Experiments) program. The coatings were exposed to atomic oxygen, space radiation, and low-orbit thermal cycling. VPS coatings showed a 56% increase in microhardness, a 26% rise in elastic modulus, minimal porosity and crack density changes compared to APS coatings. The change in mechanical properties is attributed to the formation of TiO, TiO₂ and TiN from nitrogen retention, alongside radiation-induced dislocations, which enhanced surface hardening. The oxidation of titanium led to the formation of TiO and TiO₂, while boron nitride was retained and underwent transmutation in VPS coatings. XPS and EDS analyses confirmed the enhanced space-environment resistance of VPS coatings, making them ideal for long-term spacecraft protection in lunar and Martian conditions.

Abhijith Kunneparambil Sukumaran↗

Characterization of PVD Cr, CrN, and TiN coatings on SiC

SiC ceramic matrix composites are a potential replacement for current light water nuclear reactor fuel cladding material. However, loss of fission gas via micro-cracks and corrosion remain an issue. Cathodic arc Cr, CrN, and TiN coatings were deposited on SiC tubes and plates to provide hermeticity and corrosion resistance. These coatings were characterized to determine as-deposited quality. Cross-sectional microscopy, X-ray diffraction, glow discharge optical emission spectroscopy, and scratch tests were performed to evaluate the purity, structure, and mechanical performance of the coatings. Nitride coatings had stable interfaces, but larger defects in the coatings as compared to the Cr coatings which showed cracking at the interface, but less deposition-induced defects. Despite the local state of the interface, the mechanical properties of the metallic coatings versus ceramic coatings enabled the Cr coatings to resist loads three times that of the nitride coatings during scratch tests. Finally, glow-discharge optical emission spectroscopy showed that improvement in elemental purity is needed for future coatings.

36 MATERIALS SCIENCE↗