Effects of inlet wall contour on the pressure recovery of a 10 degrees 10-inch-inlet-diameter conical diffuser
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Copp, Martin R↗
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Status Report on the Water-Based NSTF RCCS Capability: Preparations and Design for the Transformation of the Natural Convection Shutdown Heat Removal Test Facility (NSTF) From Air to Water-based Cooling
The following report provides an overview of the current status of the water-based transformation, including details of the design, geometry, and fabrication of the test section and network piping, for the ½ scale water-based NSTF program at Argonne National Laboratory. In early FY2015, efforts towards a water-based design began in parallel with on-going air-based work, and began by identifying top level objectives of the transformation. Scaling studies and preparation tasks with computational modeling were carried out to guide the design decisions, minimize distortions, and ensure relevant data among scales. This entailed close collaboration with AREVA, whose water-based RCCS (included as part of their 625 MWt SC-HTGR) served as the primary design basis for incorporation into the NSTF. A literature review of previous works was made, with an emphasis placed on similar facilities, relevance to passive decay heat removal, and details pertaining to two-phase flow and measurement techniques. The study focused on input from key designers and a thermal analysis of existing cooling panels (e.g. at TAMU and UW-Madison) and two proposed AREVA cooling panels. A base case was used as a reference point for parametric studies of effects from varying tube spacing (pitch), tube diameter, fin thickness, and materials. Then, a structural analysis was performed to ensure safe material stresses during high temperature operation. Details of the pipe network geometry and guidelines for design of the water storage tank are finally presented, followed by engineering drawings in the appendix. The results of this study have identified a suitable configuration to support both the ANL/DOE project goals and the DOE vision to provide AREVA with data suitable for characterizing the RCCS of their full scale HTGR design. The dimensions were not selected for optimal RCCS performance, but instead to serve as a representative yet bounding configuration for future implementation into a full scale design. Scaling distortions are unavoidable; however, they can be accurately predicted based on earlier works of derived similarity solutions. Flexibility remained a primary design philosophy, and will allow the test facility to easily accommodate future alterations. The final design for the test section and network piping is as follows: riser tubes: 1.5” Schedule 160, 5.91” (150-mm) pitch, 304L stainless, heat transfer panels: 5/16” plates, 4.01” (102-mm) width, full penetration weld to risers, 304L stainless, split into 4 panels per riser separated by horizontal 1/8” gaps, test section: Eight (x8) riser tubes and nine (x9) heat transfer panels, fabricated into banks of two (x2) riser tubes and three (x3) fins, joined to form single section, and network geometry: 4.0” Schedule 40, 304L stainless. Details of the water storage tank will reflect competing effects such as thermal hydraulic phenomena during single and two-phase operation. These considerations include mixing during single-phase jet penetration, condensation of rising bubbles during two-phase discharge, bubble entrainment into the liquid outlet, and liquid carry-over into the steam outlet.
22 GENERAL STUDIES OF NUCLEAR REACTORS↗
Aerosol detection efficiency in inductively coupled plasma mass spectrometry
We used an electrostatic size classification technique to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Moreover, we counted size-segregated particles with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized by the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10 -5 to 10 -11 . Free molecular heat and mass transfer theory was applied, but evaporative phenomena were not sufficient to explain the dependence of aerosol detection on particle diameter. Additional work is needed to correlate experimental data with theory for metal-oxides where thermodynamic property data are sparse relative to pure elements. Finally, when matrix effects and the diffusion of ions inside the plasma were considered, mass loading was concluded to have had an effect on the dependence of detection efficiency on particle diameter.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Tethered Formation Configurations: Meeting the Scientific Objectives of Large Aperture and Interferometric Science
With the success of the Hubble Space Telescope, it has become apparent that new frontiers of science and discovery are made every time an improvement in imaging resolution is made. For the HST working primarily in the visible and near-visible spectrum, this meant designing, building, and launching a primary mirror approximately three meters in diameter. Conventional thinking tells us that accomplishing a comparable improvement in resolution at longer wavelengths for Earth and Space Science applications requires a corresponding increase in the size of the primary mirror. For wavelengths in the sub-millimeter range, a very large telescope with an effective aperture in excess of one kilometer in diameter would be needed to obtain high quality angular resolution. Realistically a single aperture this large is practically impossible. Fortunately such large apertures can be constructed synthetically. Possibly as few as three 34 meter diameter mirrors flying in precision formation could be used to collect light at these longer wavelengths permitting not only very large virtual aperture science to be carried out, but high-resolution interferometry as well. To ensure the longest possible mission duration, a system of tethered spacecraft will be needed to mitigate the need for a great deal of propellant. A spin-stabilized, tethered formation will likely meet these requirements. Several configurations have been proposed which possibly meet the needs of the Space Science community. This paper discusses two of them, weighing the relative pros and cons of each concept. The ultimate goal being to settle on a configuration which combines the best features of structure, tethers, and formation flying to meet the ambitious requirements necessary to make future large synthetic aperture and interferometric science missions successful.
Farley, Rodger E.↗
Tethered Formation Configurations: Meeting the Scientific Objectives of Large Aperture and Interferometric Science
With the success of the Hubble Space Telescope, it has become apparent that new frontiers of science and discovery are made every time an improvement in imaging resolution is made. For the HST working primarily in the visible and near-visible spectrum, this meant designing, building and launching a primary mirror approximately three meters in diameter. Conventional thinking tells us that accomplishing a comparable improvement in resolution at longer wavelengths for Earth and Space Science applications requires a corresponding increase in the size of the primary mirror. For wavelengths in the sub-millimeter range, a very large telescope with an effective aperture in excess of one kilometer in diameter would be needed to obtain high quality angular resolution. Realistically a single aperture this large is practically impossible. Fortunately such large apertures can be constructed synthetically. Possibly as few as three 3 - 4 meter diameter mirrors flying in precision formation could be used to collect light at these longer wavelengths permitting not only very large virtual aperture science to be carried out, but high-resolution interferometry as well. To ensure the longest possible mission duration, a system of tethered spacecraft will be needed to mitigate the need for a great deal of propellant. A spin-stabilized, tethered formation will likely meet these requirements. Several configurations have been proposed which possibly meet the needs of the Space Science community. This paper discusses two of them, weighing the relative pros and cons of each concept. The ultimate goal being to settle on a configuration which combines the best features of structure, tethers and formation flying to meet the ambitious requirements necessary to make future large synthetic aperture and interferometric science missions successful.
Farley, Rodger E.↗
Effect of hydrogen on irradiation creep and growth for ZIRLO alloy and Zr-1.0Nb - 2016-0058
The impact of hydrogen on the irradiation growth and creep of stress-relief annealed (SRA) ZIRLO{sup R} alloy and recrystallized annealed (RXA) Zr-1.0Nb cladding tubes is evaluated in this paper. The samples were charged with hydrogen in the range of approximately 160-720 ppm using the gaseous method. Biaxial in-reactor creep tests were performed after Cycle 1, Cycle 2, Cycle 3, and Cycle 4, on both as received and pre-charged hydrogen cladding tubes. Outside diameter and axial length measurements were performed on the samples. The results showed that hydrogen had no effect on the axial irradiation creep but a relatively large effect on the axial irradiation growth. Increasing hydrogen decreased the axial irradiation growth in RXA Zr-1.0 Nb, which was opposite from the behavior of SRA ZIRLO cladding. This unique hydrogen effect on the irradiation axial growth of RXA Zr-1.0Nb could be due to the different intergranular stress resulting from the fabrication process or the absence of alloying elements, including tin. The total axial strain of both Zr-1.0Nb and SRA ZIRLO cladding increased with increasing fast fluence, and Zr-1.0Nb increased at a faster rate relative to SRA ZIRLO cladding. In the diameter direction, hydrogen had a minimal effect on the total diameter strain and the diameter irradiation creep strain for both SRA ZIRLO samples and the RXA Zr-1.0Nb sample. This finding from in-reactor test is contrary to the out-reactor tests results from the literature that have shown that hydrogen significantly decreases thermal creep. The total diameter strain and diameter irradiation creep behavior for the SRA ZIRLO samples and RXA Zr-1.0Nb were similar. (authors)
36 MATERIALS SCIENCE↗
Airfoil gust response and the sound produced by airifoil-vortex interaction
This paper contributes to the understanding of the noise generation process of an airfoil encountering an unsteady upwash. By using a fast Fourier transform together with accurate airfoil response functions, the lift-time waveform for an airfoil encountering a delta function gust (the indicial function) is calculated for a flat plate airfoil in a compressible flow. This shows the interesting property that the lift is constant until the generated acoustic wave reaches the trailing edge. Expressions are given for the magnitude of this constant and for the pressure distribution on the airfoil during this time interval. The case of an airfoil cutting through a line vortex is also analyzed. The pressure-time waveform in the far field is closely related to the left-time waveform for the above problem of an airfoil entering a delta function gust. The effects of varying the relevant parameters in the problem are studied, including the observed position, the core diameter of the vortex, the vortex orientation and the airfoil span. The far field sound varies significantly with observer position, illustrating the importance of non-compactness effects. Increasing the viscous core diameter tends to smooth the pressure-time waveform. For small viscous core radius and infinite span, changing the vortex orientation changes only the amplitude of the pressure-time waveform, and not the shape.
Amiet, R. K.↗
Effect of the photon lifetime on the characteristics of 850-nm vertical-cavity surface-emitting lasers with fully doped distributed Bragg reflectors and an oxide current aperture
The effect of the photon lifetime in an optical microcavity on the characteristics of 850-nm vertical-cavity surface-emitting lasers (VCSELs) with fully doped distributed Bragg reflectors (DBRs) and an oxide current aperture is studied. The photon lifetime in the microcavity is controlled by varying the upper DBR reflectance. It is found that the speed of VCSELs with a current-aperture diameter of 10 μm is mainly limited by the self-heating effect, despite an increase in the relaxation-oscillation damping coefficient with increasing photon lifetime in the microcavity. At the same time, the higher level of internal optical loss in lasers with a current-aperture diameter of 1.5 μm leads to dominance of the effect of relaxation-oscillation damping independently of the radiation output loss. In the case of devices with a current-aperture diameter of 5.5 μm, both mechanisms limiting the speed operate, which allow an increase in the VCSEL effective modulation frequency from 21 to 24 GHz as the photon lifetime decreases from 3.7 to 0.8 ps.
36 MATERIALS SCIENCE↗
Saltation threshold on Mars - The effect of interparticle force, surface roughness, and low atmospheric density
Results are reported for wind-tunnel experiments performed to determine the threshold friction speed of particles with different densities. Experimentally determined threshold speeds are plotted as a function of particle diameter and in terms of threshold parameter vs particle friction Reynolds number. The curves are compared with those of previous experiments, and an A-B curve is plotted to show differences in threshold speed due to differences in size distributions and particle shapes. Effects of particle diameter are investigated, an expression for threshold speed is derived by considering the equilibrium forces acting on a single particle, and other approximately valid expressions are evaluated. It is shown that the assumption of universality of the A-B curve is in error at very low pressures for small particles and that only predictions which take account of both Reynolds number and effects of interparticle forces yield reasonable agreement with experimental data. Effects of nonerodible surface roughness are examined, and threshold speeds computed with allowance for this factor are compared with experimental values. Threshold friction speeds on Mars are then estimated for a surface pressure of 5 mbar, taking into account all the factors considered.
Iversen, J. D.↗
An Investigation of the Effect of a Highly Favorable Pressure Gradient on Boundary-Layer Transition as Caused by Various Types of Roughnesses on a 10-foot-Diameter Hemisphere at Subsonic Speeds
Tests were made on a 10-foot-diameter hemispherical nose at Reynolds numbers up to 10 x 10(exp 6) and at a maximum Mach number of about 0.1 to determine the effects of a highly favorable pressure gradient on boundary-layer transition caused by roughness. Both two-dimensional and three-dimensional roughness particles were used, and the transition of the boundary layer was determined by hot-wire anemometers. The roughness Reynolds number for transition R(sub k,t) caused by three-dimensional particles such as Carborundum grains, spherical particles, and rimmed craters was found. The results show that for particles immersed in the boundary layer, R(sub k,t) is independent of the particle size or position on the hemispherical nose and depends mainly on the height-to-width ratio of the particle. The values of R(sub k,t) found on the hemispherical nose compare closely with those previously found on a flat plate and on airfoils with roughness. For two-dimensional roughness, the ratio of roughness height to boundary-layer displacement thickness necessary to cause transition was found to increase appreciably as the roughness was moved forward on the nose. Also included in the investigation were studies of the spread of turbulence behind a single particle of roughness and the effect of holes such as pressure orifices.
Peterson, John B., Jr.↗
Reduction of Jet Penetration in a Cross-Flow by Using Tabs
A tab placed suitably on a nozzle that produces a jet in a cross-flow can reduce the penetration of the jet. This effect, achieved when the tab is placed on the windward side of the nozzle relative to the cross flow, may be of interest in film cooling applications. Wind tunnel experiments are carried out, in the momentum ratio (J) range of 10-90, to investigate the tab geometry that would maximize this effect. The preliminary results show that a 'delta tab' having a base width approximately fifty percent of the nozzle diameter may be considered optimum. With a given tab size, the effect is more pronounced at higher J. Reduction in jet penetration by as much as 40% is observed. Comparable reduction in jet penetration is also obtained when a triangular shaped tab is placed flush with the tunnel wall or with its apex tilted down into the jet nozzle (the 'delta tab' being the configuration in which the apex is tilted up). However, the delta tab involves the least flow blockage and pressure loss. Relative to the baseline case, the lateral spreading of the jet is found to be more with the delta tab but less with other orientations of the tab.
Zaman, K. B. M. Q.↗
Effects of simulated flight on fan noise suppression
Attenuation properties of three treated fan inlets were evaluated in the NASA-Lewis Anechoic Wind Tunnel using a subsonic tip speed, 50.8 cm-diameter fan. Tunnel flow simulated the inflow clean-up effect on source noise observed in flight and allowed observation of the blade passage frequency tone cut-off phenomenon. Acoustic data consisted of isolated inlet noise measured in the far field at two positions and with traverses at four frequencies. Averaged attenuation properties showed relative agreement of the inlets with their design intent; however, tunnel flow significantly affected the attenuation spectra. With no tunnel flow the strong blade passage tone was more highly attenuated than the adjacent broadband noise. With tunnel flow, when cut-off was observed, the attenuation at the tone frequency was comparable to that for broadband noise. Tunnel flow increased by several dB the maximum attenuation occurring at midfrequencies of the attenuation spectra. The combined effect of tunnel flow on attenuation and source noise resulted in suppressed fan noise levels throughout the spectra. Tunnel flow caused some substantial directivity variations that are interpreted as acoustic mode changes, with tunnel flow generally reducing the proportion of modes near cut-off.
Heidmann, M. F.↗
Effects of aspect ratio and concentration on rheology of epoxy suspensions containing model plate-like nanoparticles
Hexagonal 2-dimensional α-zirconium phosphate crystals were prepared with lateral diameters ranging from 110 nm to 1.5 μm to investigate the effect of particle size on suspension rheology. The nanoplatelets were exfoliated to individual sheets with monodisperse thickness and dispersed in a Newtonian epoxy fluid. The steady shear response of dilute and semi-dilute suspensions was measured and compared to expressions obtained from theory for infinitely dilute suspensions. For suspensions containing the smaller nanoplatelets, aspect ratio ∼160, the low shear rate viscosity and transition to shear thinning behavior were well described by theory for loadings up to 0.5 vol. %. The agreement was improved by assuming a moderate polydispersity in lateral diameter, ∼30%–50%, which is consistent with experimental observation. For the higher aspect ratio nanoplatelets, good agreement between theory and experiment was observed only at high shear rates. At lower shear rate, theory consistently over-predicted viscosity, which was attributed to a progressive shift to non-isotropic initial conditions with increasing particle size. The results suggest that at a fixed Peclet number, there is an increasing tendency for the nanoplatelets to form transient, local stacks as particle size increases. The largest particles, aspect ratio ∼2200, showed unusual shear thinning and thickening behaviors that were attributed to particle flexibility. The findings demonstrate the surprising utility of theory for infinitely dilute suspensions to interpret, and in some cases quantitatively describe, the non-Newtonian viscosity of real suspensions containing high aspect ratio plate-like particles. A simple framework is proposed to interpret deviations from ideal behavior based on the local and collective behavior of the suspended nanoplatelets.
36 MATERIALS SCIENCE↗
Calcination pretreatment effects on acid leaching characteristics of rare earth elements from middlings and coarse refuse material associated with a bituminous coal source
The pretreatment of middlings and coarse refuse material collected from a Pocahontas No.3 coal source using calcination was investigated for the potential of improving the leaching recovery of rare earth elements. Calcination at 600 °C significantly and preferentially improved light REE (LREE) recovery to values in the range of 80-90% using 1.2 M HCl. The positive effect was due to the increased pore diameter and volume as well as thermal decomposition of the minerals associated with the LREEs. Heavy REE recovery was not increased after calcination at 600 °C due to the need for higher temperatures for the thermal decomposition of HREE minerals. Furthermore, some HREEs were also associated with sulfide minerals (e.g., pyrite) which were transformed into low-solubility oxides (e.g., hematite) after roasting at 600 °C. Based on the leaching characteristics of the major elements (Fe, Al, Ca and Mg) and REEs along with SEM EDX data, it was concluded that REEs in the two samples mainly occurred as phosphate minerals. In the middlings, some of the minerals were completely encapsulated by kaolinite, which was less apparent in the coarse refuse. In addition, it was found that a portion of the REEs (10-25%) in the samples were associated with micro-dispersed material in the organic matrix and was released after calcination and easily recovered using 0.1M (NH 4 ) 2 SO 4 solution at pH 5. In conclusion, Scandium primarily occurred in mineral forms with minimum amounts associated with ion-adsorbed clays and organic association.
01 COAL, LIGNITE, AND PEAT↗
Hydrogen adsorption and transport in clay-rich geomaterials: Implications for large-volume underground hydrogen storage
Depleted oil and gas reservoirs, characterized by impermeable clay-rich caprocks, are promising sites for large-scale underground hydrogen storage (UHS), which is a key strategy to support hydrogen-based energy systems. However, experimental data on hydrogen storage in clay-rich geomaterials remain scarce. In this work, we experimentally investigated hydrogen adsorption and migration in clay-rich geomaterials in the presence of nitrogen and water under controlled temperatures. Experimental observations showed that hydrogen was adsorbed in dry illite. A dual-porosity transport model was developed to interpret hydrogen transport between large-pore and small-pore domains in illite. The large-pore domain is the space between clay particles (i.e., inter-particle space), whereas the small-pore domain is the nanoscale pore space between clay mineral layers (i.e., inter-layer or intra-particle space). In contrast, nitrogen showed no evidence of adsorption in dry illite because it cannot move into the small-pore domain due to the relatively large kinetic diameter, referred to as the molecular sieving effect. Here, we found that 0.7–1.3 nm is the length scale regulating this molecular sieving effect, matching the interlayer spacing in illite, suggesting that nitrogen is a promising cushion gas in UHS, which aims to maintain adequate pressure in the reservoir for economic operations. In wetted illite, hydrogen was not adsorbed into the interlayer space due to the occupation of adsorption sites by interlayer water, which highlights the critical role of the clay hydration state in controlling hydrogen-clay interactions. Additionally, hydrogen adsorption experiments on crushed shale indicated that the shale surface possessed adsorption sites more favorable for hydrogen than for nitrogen. Through these experiments, we provide new insights into hydrogen storage mechanisms in clay-rich geomaterials and offer valuable laboratory data for evaluating the performance of large-scale UHS systems.
Adsorption↗
Process design of the piperazine advanced stripper for a 460 MW NGCC
The Texas Carbon Management Program is conducting a Front-End Engineering Design (FEED) for Piperazine with the Advanced Stripper™ (PZAS™) at a natural gas combined cycle power plant in west Texas. Here, this paper presents the design of the advanced stripper system with an emphasis on the selection of packing type, packing height, column diameter, and heat exchanger size, demonstrates the effect of ambient temperature swing on the regeneration energy requirement, and investigates two alternate process configurations that provide better energy performance than PZAS™. The design uses 2 stripper trains, and each train uses two cold cross exchangers, one hot cross exchanger, a stripper column, a CO 2 exchanger, and a condenser. Each column consists of two sections of random packing with RSR 2 packing at the top and RSR 3 packing at the bottom, with a total packed height of 7.5 m. The cold exchanger was designed with an NTU of 6, the hot exchanger with an NTU of 2, and the CO 2 exchanger with an NTU of 5. At 0.4 rich loading and 0.2 lean loading, this design resulted in a heat duty of 2.85 GJ/tonne CO 2 . The heat duty can vary up to 3.1 GJ/tonne CO 2 due to lower rich loading at higher summer temperature, but the absolute steam requirement is 8–15% lower in the summer. An alternate design, PZAS with hot rich bypass, is proposed, which can reduce the equivalent work of stripping by 1.5–3.5% compared to PZAS at low heat exchanger size, due to a reduction in stripper driving force. Using a hot rich bypass increases the vapor fraction of the total rich bypass stream from 0.3 to 1 mol% compared to using the warm rich bypass, which also contributes to a reduction in lost work in the column. PZAS with hot rich bypass outperforms PZAS in energy requirement below a packing height of 15 m, but fails to do so above 15 m of packing due to a column pinch that results in little change in LMTD of the column. PZAS with hot rich bypass has the potential to minimize capital cost in addition to reducing energy requirement as it requires less packing to strip CO 2 than PZAS and requires only one cross exchanger with 8 heat transfer units.
03 NATURAL GAS↗
Effect of micro-fin tube geometry parameters on evaporator material savings
A Performance Evaluation Criteria (PEC) analysis is presented that explores the influence of the micro-fin tube geometry on the required material volume. The analysis was done using a local flow boiling model, which can quantify the effect of fin parameters and the tube diameter. The PEC was done while requiring that the compared surfaces satisfy the same heat duty and pressure drop. The following tube parameters and ranges were explored: tube diameter (3 mm ≤ D o ≤ 6 mm), fin base thickness (0.12 mm ≤ t bf ≤ 0.29 mm), helix angle (6° ≤ α ≤ 30°), fin apex angle (11° ≤ β ≤ 22°), total number of fins (43 ≤ n f ≤ 70), and the fin height (0.11 mm ≤ e ≤ 0.3 mm). The tube that provided the smallest material requirements within the examined parameter ranges had: D o = 3 mm, t bf = 0.12 mm, α = 6°, β = 11°, n f = 43, and e = 0.3 mm. In general, small D o and t bf and large n f and e provided the best performance and work to minimize the required material volume to provide a given heat duty and pressure drop. The helix and the fin-tip apex angles were found to have very little influence on the performance for the examined range of parameters and angles associated with the lowest production cost should be chosen.
Evaporation↗
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↗