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At least 19 records

Vertically oriented ZrO 2 –TiO 2 –Nb 2 O 5 –Al 2 O 3 mixed nanopatterned bioceramics on Ti6Al7Nb implant assessed by laser spallation technique

Recently, reports on the fabrication of nonstructural configuration have generated scientific interest due to increased awareness of the oxide nanotubes in the biomedical implant field and other industrial approaches. In this paper, highly ordered ZrO 2 –TiO 2 –Nb 2 O 5 –Al 2 O 3 nanotube arrays were grown by physical vapor deposition (PVD) of a zirconium layer on titanium-niobium alloy implant (IMPTi67) and succeeding anodic oxidation at a constant voltage (60 V) with exposure times ranging from 30 to 300 min. To crystallize the resulting mixed oxide nanotubes, heat treatment was also applied. The nanotubes were placed in an atmospheric furnace at temperatures ranging from 450 to 800 °C for 2 h. This treatment provided a morphological evolution was strongly influenced by the anodization time, where highly aligned bamboo-shaped oxide nanotubes (161 ± 44 nm in inside diameter and ~1 μm in length) were formed after 300 min of anodization. After annealing at temperature below 500 °C, the nano-array configuration remained stable and the average inner diameter decreased to around 40 nm. The effects of anodically fabrication time on the adhesion strength of four-phase multilayered mixed oxide nanotubes on anodized Zr/IMPTi67 surfaces assed by microscratch analysis. From the results, increasing the annealing temperature further to 800 °C fully destroyed the nanotubes and consequently the tubular arrangement was converted to a coarse grain structure. It was revealed that annealing at 450 °C for 2 h was the optimum conditions for stable nanotubular array generation, where the highest adhesion strength (shifted from 2595.59 to 2640.12 mN), microhardness (372 HV) and hydrophilicity (15 ± 1°) were recorded. It is notify that the adhesion strength of highly ordered mixed nanotubes was remarkably decreased after thermal treatment at 800 °C (1817.51 mN). Through the laser spallation analysis, the intrinsic adhesion strength of the Zr/IMPTi67 interface was found to be at 63 MPa, while the first stages of failure occurred at a stress state of 35 MPa. The adhesion of the film with the tubular structure proved to have a significantly larger adhesion strength of 246 MPa for the complete failure and 203 MPa for incipient stages of spallation. Finally, the considered surface modification can be an effective step in determining the interface strength between biomedical implants and the nanostructured coatings.

36 MATERIALS SCIENCE↗

Adhesion measurement of highly-ordered TiO 2 nanotubes on Ti-6Al-4V alloy

Self-assembled nanotubular arrays on Ti alloys could be used for more effective implantable devices in various medical approaches. In the present work, the adhesion of TiO 2 nanotubes (TiO 2 NTs) on Ti-6Al-4V (Ti64) was investigated by laser spallation and scratch test techniques. At first, electrochemical anodization was performed in an ammonium fluoride solution dissolved in a 90:10 ethane-1,2-diol (ethylene glycol) and water solvent mixture. This process was performed at room temperature (23 °C) at a steady potential of 60 V for 1 h. Next, the TiO 2 nanotubes layer was heat-treated to improve the adhesion of the coating. The formation of self-organized TiO 2 nanotubes as well as the microstructural evolution, are strongly dependent on the processing parameters and subsequent annealing. From microscopic analysis, highly oriented arrays of TiO 2 nanotubes were grown by thermal treatment for 90 min at 500 °C. Further heat treatment above 500 °C led to the detachment of the nanotubes and the complete destruction of the nanotubes occurred at temperature above 700 °C. Scratch test analysis over a constant scratch length (1000 μm) indicated that the failure point was shifted from 247.4 to 557.9 μm while the adhesion strength was increased from ~862 to ~1814 mN after annealing at 500 °C. Finally, the adhesion measurement determined by laser spallation technique provided an intrinsic adhesion strength of 51.4 MPa for the TiO 2 nanotubes on the Ti64 substrate.

36 MATERIALS SCIENCE↗

Robustness and printed sensor qualification

A limiting factor of additive manufactured (AM) sensors for in-pile applications is the development of appropriate interconnection and packaging strategies that can maintain reliable performance in extreme environments. Failure mechanisms in these harsh conditions could include, but not limited to, materials interaction (i.e., intermetallic formation) and coefficient of thermal expansion (CTE) mismatch between the individual components of the sensors. To mitigate premature failure and enable the successful sustained operation of AM sensors, non-destructive qualification tests are used as an intermediate process control step used for verifying robustness and reliability of the sensor before they are deployed. A materials system of interest is the use of barium strontium titanium oxide (BST) films on stainless steel 316L (SS316L) substrate. Due to BST’s high dielectric constant and tunable dielectric properties, there is an interest for its application as an insulation/encapsulation layer for capacitive strain gauges when printed on structural materials. Previous work on the BST/SS316L material system, however, showed that the BST cracks when exposed to temperatures up to 600 °C due to CTE mismatch between the printed BST film and the metallic substrate. When comparing different fabrication techniques, less surface cracking was observed in the samples that deposited thinner (i.e., 2-20 μm) than samples that were thicker (i.e., 135 µm – 300 µm). The objective of this report is to establish a qualification process that will determine and address any challenges (i.e., mechanical failure of thick prints) of the AM sensor prior to its application in experimental tests. To demonstrate the qualification process in this report, laser spallation and uniaxial tensile tests using dynamic and quasi-static loading, respectively, will be discussed.

36 - MATERIALS SCIENCE↗

Dynamics of spallation during femtosecond laser ablation studied by time-resolved reflectivity with double pump pulses

The dynamics of photomechanical spallation during femtosecond laser ablation of fused silica was studied by time-resolved reflectivity with double pump pulses. Oscillation of reflectivity was caused by interference between the probe pulses reflected at the sample surface and the spallation layer, and was enhanced when the surface was irradiated with the second pump pulse within a time interval, Δτ, of several picoseconds after the first pump pulse. However, as Δτ was increased, the oscillation amplitude decreased with an exponential decay time of 10 ps. The oscillation disappeared when Δτ exceeded 20 ps. This result suggests that the formation time of the spallation layer is approximately 10 ps. A second pump pulse with Δτ shorter than 10 ps excites the bulk sample. The spallation layer that is photo-excited by the first and second pump pulses is separated afterward. In contrast, a pulse with Δτ longer than the formation time excites and breaks up the spallation layer that has already been separated from the bulk. The formation time of the spallation layer, as determined in this experiment, is attributed to the characteristic time of the mechanical equilibration corresponding to the thickness divided by the sound velocity of the photo-excited layer.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Generation of nanocrystalline surface layer in short pulse laser processing of metal targets under conditions of spatial confinement by solid or liquid overlayer

The effect of spatial confinement by a solid or liquid overlayer on short pulse laser-induced surface microstructure modification is investigated in a series of large-scale atomistic simulations performed for Ag targets irradiated in the regime of melting and resolidification, below the thresholds for laser spallation and ablation. For Ag targets with free surfaces, the formation of a nanocrystalline region with random crystallographic grain orientation is observed under irradiation conditions leading to the generation of numerous sub-surface voids that slow down the solidification process. When no voids are generated, the resolidification produces grains misoriented with respect to the bulk of the target by just several degrees and separated from each other by low angle grain boundaries or dislocation walls. The presence of a liquid or solid overlayer suppresses nucleation of sub-surface voids, provides an additional pathway for cooling through the heat conduction to the overlayer, and facilitates the formation of nanocrystalline structure in a region of the metal target adjacent to the overlayer. Moreover, the stabilizing effect of the solid overlayer may result in an incomplete melting of metal in the vicinity of the interface, making it possible for grains growing from the interface to retain “memory” of the target orientation and to produce nanocrystalline interfacial region with small misorientation of grains with respect to the bulk of the target. In all simulations, the nanocrystalline layers generated by laser processing of single crystal Ag targets are characterized by a high density of stacking faults, twin boundaries, and point defects produced in the course of the rapid resolidification.

Chemistry↗

Generation of negative pressures and spallation phenomena in diamond exposed to a picosecond laser pulse

The spallation phenomena in poly- and single-crystal synthetic diamonds have been experimentally investigated. A shockwave impact on a target was implemented using a 70-ps laser pulse in the Kamerton-T facility. The ablation pressure of 0.66 TPa on the front target surface was formed by pulsed radiation of a neodymium phosphate glass laser (second harmonic λ = 0.527 mm, pulse energy 2.5 J) with an intensity as high as 2 × 10{sup 13} W cm{sup -2}. The maximum diamond spall strength σ* ≈ 16.5 GPa is found to be 24% of the theoretical ultimate strength. Raman scattering data indicate that a small amount of crystalline diamond in the spallation region on the rear side of the target is graphitised. (extreme light fields and their applications)

43 PARTICLE ACCELERATORS↗

Adhesion Testing of Direct-Write Printed Ink on Metallic Structural Components

The successful adoption of additive manufacturing for the rapid prototyping of direct-write printed electronics requires the establishment of quantifiable metrics that can interrogate device performance. One measure of performance is the adhesion strength between the substrate and printed film interface, which is critical since the strength of this interface can dictate the accuracy and reliability of the printed device. In this work, a non-contact laser-induced spallation technique was used to quantify the adhesion of silver printed films on aluminum alloy substrates. The laser-based method was compared to a standardized pull-off adhesion test, which provided baseline measurements of adhesion strength. The sintering conditions were shown to play an important role in the film-substrate adhesion strength, as well as the cohesion and ductility of the film itself. The methods and results described in this work support the establishment of process control steps that are necessary for quickly verifying the reliability of printed devices prior to their deployment in critical experiments.

Adhesion test↗

Development of Quality Control Methods for Robust and Reliable Sensor Design

The successful adoption of additive manufacturing for the rapid prototyping of printed sensors requires the establishment of quantifiable metrics that can interrogate device performance. One measure of performance is the adhesion strength between the substrate and sensor interface, which is critical since the strength of this interface can dictate the accuracy and reliability of the printed sensor. In this work, a non-contact laser-induced spallation technique was used to quantify the adhesion of silver prints on an aluminum alloy substrate. The laser-based method was compared to a standardized pull-off adhesion test, which provided baseline measurements of adhesion strength. The sintering conditions were shown to play an important role in the film-substrate adhesion strength, as well as the cohesion and ductility of the film itself. The methods and results described in this work supports the establishment of process control steps that are necessary for verifying the reliability of printed devices prior to its deployment in critical experiments.

36 MATERIALS SCIENCE↗

Advanced Manufactured Strain Sensors for Extreme Environments

Experimentation at irradiation test facilities are essential for reducing the innovation time of developmental fuels, fuel cladding, and structural materials employed in next-generation nuclear reactors. However, due to the harsh conditions generated in such reactors and limited instrumentation space, the evaluation of a material’s mechanical properties is often limited to characterization after the materials have been removed from reactor conditions, or post-irradiation examination. These experiments are costly, time-consuming, and fail to capture the critical time-evolving phenomena that occur during the irradiation experiments. Advanced manufactured digital image correlation patterns and strain sensor devices serve as two promising technologies that can be deployed in the confined and challenging orientations of these irradiation experiments while also providing key insight on salient materials phenomena (i.e., mechanical properties).To guide the development of the printed strain sensors prior to their deployment in critical experiments, the adhesion strength between the substrate and printed film interface is measured via tensile testing and a non-contact laser-induced spallation technique. The establishment of these process control steps helped guide the successful fabrication and testing of direct-write strain sensing devices discussed in this work. The fabrication process controls are necessary for enabling the sustained operation of these strain sensing device through experimentation and minimize the potential for premature failure.

36 - MATERIALS SCIENCE↗

Laser-based Adhesion Strength Measurements for Advanced Manufactured Sensor Adhesion Characterization

As part of the advanced manufacturing (AM) focus of the Nuclear Energy Enabling Technologies (NEET) Advanced Sensors and Instrumentation (ASI) Program, new in-house capabilities to fabricate and test novel active and passive in-pile sensors are being developed at the Idaho National Laboratory (INL). These advanced-manufactured sensors, such as peak temperature monitors and strain gauges, must be miniaturized and be able to provide real-time feedback, all while withstanding the coupled extremes of temperature and radiation typically observed in the environment of a nuclear test reactor. Fabricating durable and robust in-pile sensors with high fidelity requires a fundamental understanding of the optimal process parameters required in the AM technique, as well as the effect of deviations from optimal process parameters on the sensor-substrate adhesion and the ultimate robustness of the sensor. This report presents the use of a laser-based, non-contact approach for characterizing the adhesion of sensors manufactured using aerosol jet printing (AJP) that comprise of silver nanoparticle inks deposited and sintered on austenitic stainless steel (SS) 316L substrates. The effect of substrate surface roughness, surface energy, ink sintering time and sintering temperature on the printed sensor topography and the sensor-substrate adhesion has been systematically investigated. The sensor-substrate interfacial adhesion strength was determined from the critical laser pulse energy required to ablate/ detach the printed sensor from the substrate. Measurements of the sensor topography using optical profilometry revealed that post-deposition sintering at 400°C for 60 minutes resulted in a reduced sensor thickness, while plasma treating the substrate prior to printing yielded sensors with uniform thickness profiles transverse to the print direction. Sintering temperature and time were found to be the dominant parameters that affected sensor-substrate adhesion, followed by substrate surface roughness. The laser-based and locally-destructive approach for adhesion strength measurements shows promise in overcoming the challenges and limitations of current standardized peel tests and can be developed into a post-fabrication process control protocol for evaluating the durability of AM printed sensors in a high throughput fashion. Future studies will investigate the use of laser-induced spallation techniques as well as non-destructive laser ultrasonic methods for sensor-substrate adhesion characterization on sensors manufactured using AJP and other AM techniques such as plasma jet printing (PJP).

42 ENGINEERING↗

Laser lift-off scribing of the CZTSe thin-film solar cells at different pulse durations

Here, the transition to fully sized solar modules requires additional three-step laser structuring processes to preserve small-scale cell efficiencies over the large areas. The adjacent cell isolation (the P3 scribe) was found to be the most sensitive process in the case of laser induced damage. The laser induced layer lift-off mechanism seems to be a very attractive process for the P3 patterning, since almost all the laser affected material is removed by mechanical spallation. However, a laser induced layer spallation behavior together with scribe electrical validation under the different laser pulse durations was not investigated extensively in the past. Therefore, we report our novel results on the P2 and P3 laser lift-off processing of the Cu 2 ZnSn(S, Se 4 ) (CZTSe) thin-film solar cells covering the pulse duration range from 300 fs to 60 ps. Shorter sub-ps pulses enabled us to process smaller P2 and P3 craters, although the lift-off threshold fluences were higher compared to the longer ps pulses. In the case of the layer lift-off, the laser radiation had to penetrate through the layer stack down to the CZTSe/Mo interface. At shorter sub-ps pulses, the nonlinear effects triggered absorption of the laser radiation in the bulk of the material, resulting in increased damage of the CZTSe layer. The Raman measurements confirmed the CZTSe surface stoichiometry changes for shorter pulses. Furthermore, shorter pulses induced higher electrical conductivity of a scribe, resulting in lower photo-electrical efficiency during the mini-module simulation. In the case of the P3 lift-off scribing, the 10 ps pulses were more favorable than shorter femtosecond pulses.

14 SOLAR ENERGY↗

Advanced Manufactured Strain Sensors for Extreme Environments

Experimentation at irradiation test facilities are essential for reducing the innovation time of developmental fuels, fuel cladding, and structural materials employed in next-generation nuclear reactors. However, due to the harsh conditions generated in such reactors and limited instrumentation space, the evaluation of a material’s mechanical properties is often limited to characterization after the materials have been removed from reactor conditions, or post-irradiation examination. These experiments are costly, time-consuming, and fail to capture the critical time-evolving phenomena that occur during the irradiation experiments. Advanced manufactured digital image correlation patterns and strain sensor devices serve as two promising technologies that can be deployed in the confined and challenging orientations of these irradiation experiments while also providing key insight on salient materials phenomena (i.e., mechanical properties). To guide the development of the printed strain sensors prior to their deployment in critical experiments, the adhesion strength between the substrate and printed film interface is measured via tensile testing and a non-contact laser-induced spallation technique. The establishment of these process control steps helped guide the successful fabrication and testing of direct-write strain sensing devices discussed in this work. The fabrication process controls are necessary for enabling the sustained operation of these strain sensing device through experimentation and minimize the potential for premature failure.

36 - MATERIALS SCIENCE↗

Negative pressure and spallation in graphite targets under nano- and picosecond laser irradiation

We present the results of experiments on the spallation phenomena in graphite targets under shock-wave nano- and picosecond irradiation, which have been performed on Kamerton-T (GPI, Moscow, Russia) and PHELIX (GSI, Darmstadt, Germany) laser facilities. In the range of the strain rates of 10{sup 6} – 10{sup 7} s{sup -1}, the data on the dynamic mechanical strength of the material at rapure (spallation) have been for the first time obtained. With a maximal strain rate of 1.4 × 10{sup 7} s{sup -1}, the spall strength of 2.1 GPa is obtained, which constitutes 64% of the theoretical ultimate tensile strength of graphite. The effect of spallation is observed not only on the rear side of the target, but also on its irradiated (front) surface. With the use of optical and scanning electron microscopes, the morphology of the front and rear surfaces of the targets is studied. By means of Raman scattering of light, the graphite structure both on the target front surface under laser exposure and on its rear side in the spall zone is investigated. A comparison of the dynamic strength of graphite and synthetic diamond is performed. (extreme light fields and their applications)

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Shock compression response of additively manufactured AlSi10Mg

We measured the Hugoniot, Hugoniot elastic limit (HEL), and spallation strength of laser powder bed fusion (LPBF) AlSi10Mg via uniaxial plate-impact experiments to stresses greater than 13 GPa. Despite its complex anisotropic microstructure, the LPBF AlSi10Mg did not exhibit significant orientation dependence or sample-to-sample variability in these measured quantities. We found that the Hugoniot response of the LPBF AlSi10Mg is similar to that of other Al-based alloys and is well approximated by a linear relationship: u s = 5.49 + 1.39u p . Additionally, the measured HELs ranged from 0.25 to 0.30 GPa and spallation strengths ranged from 1.16 to 1.45 GPa, consistent with values reported in other studies of LPBF AlSi10Mg and Al-based alloys. Furthermore, strain-rate and stress dependence of the spallation strength were also observed.

36 MATERIALS SCIENCE↗

Jet formation in spallation of metal film from substrate under action of femtosecond laser pulse

It is well known that during ablation by an ultrashort laser pulse, the main contribution to ablation of the substance is determined not by evaporation, but by the thermomechanical spallation of the substance. For identical metals and pulse parameters, the type of spallation is determined by film thickness d{sub f}. An important gauge is metal heating depth d{sub T} at the two-temperature stage, at which electron temperature is higher than ion temperature. We compare cases with d{sub f} < d{sub T} (thin film) and d{sub f} ≫ d{sub T} (bulk target). Radius R{sub L} of the spot of heating by an optical laser is the next (after d{sub f}) important geometrical parameter. The morphology of film bulging in cases where d{sub f} < d{sub T} on the substrate (blistering) changes upon a change in radius R{sub L} in the range from diffraction limit R{sub L} ∼ λ to high values of R{sub L} ≫ λ, where λ ∼ 1 μm is the wavelength of optical laser radiation. When d{sub f} < d{sub T}, R{sub L} ∼ λ, and F{sub abs} > F{sub m}, gold film deposited on the glass target acquires a cupola-shaped blister with a miniature frozen nanojet in the form of a tip on the circular top of the cupola (F{sub abs} and F{sub m} are the absorbed energy and the melting threshold of the film per unit surface area of the film). A new physical mechanism leading to the formation of the nanojet is proposed.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Workshop on laser-driven neutron sources held at LANSCE

A workshop on laser-driven neutron sources was held at the Los Alamos Neutron Science Center (LANSCE), Los Alamos, New Mexico USA, on August 16th, 2017. The workshop brought together experts in plasma physics, high intensity lasers, laser target fabrication, spallation physics, and applications for intense pulsed neutron sources.

07 ISOTOPE AND RADIATION SOURCES↗

Spallation-induced roughness promoting high spatial frequency nanostructure formation on Cr

Interaction of ultrafast laser pulses with metal surfaces in the spallation regime can result in the formation of anisotropic nanoscale surface morphology commonly referred to as laser-induced periodic surface structures (LIPSS) or ripples. The surface structures generated by a single pulse irradiation of monocrystalline Cr samples are investigated experimentally and computationally for laser fluences that produce high spatial frequency nanostructures in the multi-pulse irradiation regime. Electron microscopy reveals distinct response of samples with different crystallographic surface orientations, with (100) surfaces exhibiting the formation of more refined nanostructure by a single pulse irradiation and a more pronounced LIPSS after two laser pulses as compared to (110) surfaces. A large-scale molecular dynamics simulation of laser interaction with a (100) Cr target provides detailed information on processes responsible for spallation of a liquid layer, redistribution of molten material, and rapid resolidification of the target. The nanoscale roughness of the resolidified surface predicted in the simulation features elongated frozen nanospikes, nanorims and nanocavities with dimensions and surface density similar to those in the surface morphology observed for (100) Cr target with atomic force microscopy. The results of the simulation suggest that the types, sizes and dimensions of the nanoscale surface features are defined by the competition between the evolution of transient liquid structures generated in the spallation process and the rapid resolidification of the surface region of the target. The spallation-induced roughness is likely to play a key role in triggering the generation of high-frequency LIPSS upon irradiation by multiple laser pulses.

Materials Science↗

Understanding the plasticity contributions during laser-shock loading and spall failure of Cu microstructures at the atomic scales

A hybrid atomic-scale and continuum modeling framework is used to study the microstructural evolution during the laser-induced shock deformation and failure (spallation) of copper microstructures. A continuum two-temperature model (TTM) is used to account for the interaction of Cu atoms with a laser in molecular dynamics (MD) simulations. The MD-TTM simulations study the effect of laser loading conditions (laser fluence) on the microstructure (defects) evolution during various stages of shock wave propagation, reflection, and interaction in single-crystal (sc) Cu systems. In addition, the role of the microstructure is investigated by comparing the defect evolution and spall response of sc-Cu and nanocrystalline (nc) Cu systems. The defect (stacking faults and twin faults) evolution behavior in the metal at various times is further characterized using virtual in situ selected area electron diffraction and x-ray diffraction during various stages of evolution of microstructure. Here, the simulations elucidate the uncertain relation between spall strength and strain-rate and the much stronger relation between the spall strength and the temperatures generated due to laser shock loading for the small Cu sample dimensions considered here.

36 MATERIALS SCIENCE↗