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At least 19 records

Test surfaces useful for calibration of surface profilometers

The present invention provides for test surfaces and methods for calibration of surface profilometers, including interferometric and atomic force microscopes. Calibration is performed using a specially designed test surface, or the Binary Pseudo-random (BPR) grating (array). Utilizing the BPR grating (array) to measure the power spectral density (PSD) spectrum, the profilometer is calibrated by determining the instrumental modulation transfer.

47 OTHER INSTRUMENTATION↗

Calibration of the modulation transfer function of surface profilometers with binary pseudo-random test standards: expanding the application range

A modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays [Proc. SPIE 7077-7 (2007), Opt. Eng. 47, 073602 (2008)] has been proven to be an effective MTF calibration method for a number of interferometric microscopes and a scatterometer [Nucl. Instr. and Meth. A616, 172 (2010)]. Here we report on a further expansion of the application range of the method. We describe the MTF calibration of a 6 inch phase shifting Fizeau interferometer. Beyond providing a direct measurement of the interferometer's MTF, tests with a BPR array surface have revealed an asymmetry in the instrument's data processing algorithm that fundamentally limits its bandwidth. Moreover, the tests have illustrated the effects of the instrument's detrending and filtering procedures on power spectral density measurements. The details of the development of a BPR test sample suitable for calibration of scanning and transmission electron microscopes are also presented. Such a test sample is realized as a multilayer structure with the layer thicknesses of two materials corresponding to BPR sequence. The investigations confirm the universal character of the method that makes it applicable to a large variety of metrology instrumentation with spatial wavelength bandwidths from a few nanometers to hundreds of millimeters.

42 ENGINEERING↗

Calibration of the modulation transfer function of surface profilometers with binary pseudo-random test standards: Expanding the application range

A modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays [Proc. SPIE 7077-7 (2007), Opt. Eng. 47(7), 073602-1-5 (2008)] has been proven to be an effective MTF calibration method for a number of interferometric microscopes and a scatterometer [Nucl. Instr. and Meth. A 616, 172-82 (2010]. Here we report on a significant expansion of the application range of the method. We describe the MTF calibration of a 6 inch phase shifting Fizeau interferometer. Beyond providing a direct measurement of the interferometer's MTF, tests with a BPR array surface have revealed an asymmetry in the instrument's data processing algorithm that fundamentally limits its bandwidth. Moreover, the tests have illustrated the effects of the instrument's detrending and filtering procedures on power spectral density measurements. The details of the development of a BPR test sample suitable for calibration of scanning and transmission electron microscopes are also presented. Such a test sample is realized as a multilayer structure with the layer thicknesses of two materials corresponding to BPR sequence. The investigations confirm the universal character of the method that makes it applicable to a large variety of metrology instrumentation with spatial wavelength bandwidths from a few nanometers to hundreds of millimeters.

47 OTHER INSTRUMENTATION↗

Calibration of the Modulation Transfer Function of Surface Profilometers with Binary Pseudorandom Test Standards: Expanding the Application Range to Fizeau Interferometers and Electron Microscopes

A modulation transfer function (MTF) calibration method based on binary pseudorandom (BPR) gratings and arrays has been proven to be an effective MTF calibration method for interferometric microscopes and a scatterometer. Here we report on a further expansion of the application range of the method. We describe the MTF calibration of a 6 in. phase shifting Fizeau interferometer. Beyond providing a direct measurement of the interferometer's MTF, tests with a BPR array surface have revealed an asymmetry in the instrument's data processing algorithm that fundamentally limits its bandwidth. Moreover, the tests have illustrated the effects of the instrument's detrending and filtering procedures on power spectral density measurements. The details of the development of a BPR test sample suitable for calibration of scanning and transmission electron microscopes are also presented. Such a test sample is realized as a multilayer structure with the layer thicknesses of two materials corresponding to the BPR sequence. The investigations confirm the universal character of the method that makes it applicable to a large variety of metrology instrumentation with spatial wavelength bandwidths from a few nanometers to hundreds of millimeters.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Characterization of electron microscopes with binary pseudo-random multilayer test samples

Verification of the reliability of metrology data from high quality x-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays has been suggested [Proc. SPIE 7077-7 (2007), Opt. Eng. 47(7), 073602-1-5 (2008)} and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer [Nucl. Instr. and Meth. A 616, 172-82 (2010)]. Here we describe the details of development of binary pseudo-random multilayer (BPRML) test samples suitable for characterization of scanning (SEM) and transmission (TEM) electron microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi2/Si multilayer coating with pseudo randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize x-ray microscopes. Corresponding work with x-ray microscopes is in progress.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Designing Pulse Laser Surface Modification of H13 Steel Using Response Surface Method

This paper presents a design of experiment (DOE) for laser surface modification process of AISI H13 tool steel in achieving the maximum hardness and minimum surface roughness at a range of modified layer depth. A Rofin DC-015 diffusion-cooled CO{sub 2} slab laser was used to process AISI H13 tool steel samples. Samples of 10 mm diameter were sectioned to 100 mm length in order to process a predefined circumferential area. The parameters selected for examination were laser peak power, overlap percentage and pulse repetition frequency (PRF). The response surface method with Box-Behnken design approach in Design Expert 7 software was used to design the H13 laser surface modification process. Metallographic study and image analysis were done to measure the modified layer depth. The modified surface roughness was measured using two-dimensional surface profilometer. The correlation of the three laser processing parameters and the modified surface properties was specified by plotting three-dimensional graph. The hardness properties were tested at 981 mN force. From metallographic study, the laser modified surface depth was between 37 {mu}m and 150 {mu}m. The average surface roughness recorded from the 2D profilometry was at a minimum value of 1.8 {mu}m. The maximum hardness achieved was between 728 and 905 HV{sub 0.1}. These findings are significant to modern development of hard coatings for wear resistant applications.

36 MATERIALS SCIENCE↗

Deposition and characterization of diamond thin films by HF-CVD method

Effect of reactor pressure and methane gas concentration on the growth of diamond films on Si (100) substrate by hot filament chemical vapor deposition (HFCVD) method has been studied in this work. Raman spectroscopy measurements of the obtained film confirmed the formation of a mixture of micro and nanocrystalline diamond by showing peaks at 1140 and 1334 cm{sup −1} wave shifts. Scanning electron microscopy results showed formation of well defined faceted diamond grains of 100–500 nm size. Average roughness of the films measured by a surface profilometer was in the range of 40–60 nm.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Zinc Oxide Thin Films Fabricated with Direct Current Magnetron Sputtering Deposition Technique

Zinc oxide (ZnO) is a very promising material for emerging large area electronic applications including thin-film sensors, transistors and solar cells. We fabricated ZnO thin films by employing direct current (DC) magnetron sputtering deposition technique. ZnO films with different thicknesses ranging from 100 nm to 1020 nm were deposited on silicon (Si) substrate. The deposition pressure was varied from 12 mTorr to 25 mTorr. The influences of the film thickness and the deposition pressure on structural properties of the ZnO films were investigated using Mahr surface profilometer and atomic force microscopy (AFM). The experimental results reveal that the film thickness and the deposition pressure play significant role in the structural formation of the deposited ZnO thin films. ZnO films deposited on Si substrates are promising for variety of thin-film sensor applications.

36 MATERIALS SCIENCE↗

Effect of RF power and annealing on chemical bonding and morphology of a-CN{sub x} thin films as humidity sensor

Amorphous carbon nitride (a-CN{sub x}) thin films were deposited using radio frequency plasma enhanced chemical vapor deposition (rf-PECVD) technique. A set of a-CN{sub x} thin films were prepared using pure methane (CH{sub 4}) gas diluted with nitrogen (N{sub 2}) gas. The rf power was varied at 50, 60, 70, 80, 90 and 100 W. These films were then annealed at 400 °C in a quartz tube furnace in argon (Ar) gas. The effects of rf power and thermal annealing on the chemical bonding and morphology of these samples were studied. Surface profilometer was used to measure film thickness. Fourier transform infra-red spectroscopy (FTIR) and Field emission scanning electron microscopy (FESEM) measurements were used to determine their chemical bonding and morphology respectively. The deposition rate of the films increased constantly with increasing rf power up to 80W, before decreasing with further increase in rf power. Fourier transform infra-red spectroscopy (FTIR) studies showed a systematic change in the spectra and revealed three main peaks included C-N, C=N, C=C and C≡N triple bond. C=N and C≡N bonds decreased with increased C-N bonds after thermal annealing process. The FESEM images showed that the structure is porous for as-deposited and covered by granule-like grain structure after thermal annealing process was done. The resistance of the a-CN{sub x} thin film changed from 23.765 kΩ to 5.845 kΩ in the relative humidity range of 5 to 92 % and the film shows a good response and repeatability as a humidity sensing materials. This work showed that rf power and thermal annealing has significant effects on the chemical bonding and surface morphology of the a-CN{sub x} films and but yield films which are potential candidate as humidity sensor device.

36 MATERIALS SCIENCE↗

Effects of Co{sub 3}O{sub 4} Addition on Friction and Dry Sliding Wear Characteristics of 8 mol% Yttria-Stabilized Cubic Zirconia

The aim of the present study was to investigate the influence of Co{sub 3}O{sub 4} additive on the microstructure, wear, and tribological properties of 8 mol% yttria-stabilized cubic zirconia (8YSZ) using a pin-on-disk tribometer, surface profilometer, hardness tester, and a scanning electron microscopy system. Specimens were produced by doping 1-15 wt.% Co{sub 3}O{sub 4} in 8YSZ using a colloidal process, sintering at 1500 °C for 1 h, and subsequent annealing at 1500 °C for 10 and 50 h. Microstructural analysis showed that Co{sub 3}O{sub 4} dissolved partially in 8YSZ, with the undissolved Co{sub 3}O{sub 4} precipitating as a secondary phase at the grain boundaries. Further, the addition of Co{sub 3}O{sub 4} enhanced the grain size. Wear tests were carried out using an Al{sub 2}O{sub 3} ball as the counterface against ceramic disk under dry sliding friction conditions at room temperature (24 °C). The wear volume of 8YSZ decreased from 0.30 to 0.11 mm{sup 3} as a result of the addition of 15 wt.% Co{sub 3}O{sub 4}. Additionally, friction coefficient of the 8YSZ significantly reduced from 0.55 to 0.17 at the beginning stage of the sliding after the addition of 15 wt.% Co{sub 3}O{sub 4}. This was because Co{sub 3}O{sub 4} creates a thin lubricating layer on the friction surface. In addition, the undoped and Co{sub 3}O{sub 4}-doped 8YSZ specimens exhibited abrasive wear under the dry sliding friction conditions, owing to the formation and propagation of microcracks, which resulted in the removal of material from the surface. The specific wear rate of 8YSZ decreased with increasing the Co{sub 3}O{sub 4} content. Thus, the addition of Co{sub 3}O{sub 4} to 8YSZ improves its wear resistance and surface topography.

36 MATERIALS SCIENCE↗

Characterization of Electron Microscopes with Binary Pseudo-random Multilayer Test Samples

Verification of the reliability of metrology data from high quality X-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binary pseudo-random (BPR) gratings and arrays has been suggested [1] and [2] and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer [5]. Here we describe the details of development of binary pseudo-random multilayer (BPRML) test samples suitable for characterization of scanning (SEM) and transmission (TEM) electron microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi2/Si multilayer coating with pseudo-randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML test samples can be used to characterize X-ray microscopes. Corresponding work with X-ray microscopes is in progress.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Transfer of autocollimator calibration for use with scanning gantry profilometers for accurate determination of surface slope and curvature of state-of-the-art x-ray mirrors

X-ray optics, desired for beamlines at free-electron-laser and diffraction-limited-storage-ring x-ray light sources, must have almost perfect surfaces, capable of delivering light to experiments without significant degradation of brightness and coherence. To accurately characterize such optics at an optical metrology lab, two basic types of surface slope profilometers are used: The long trace profilers (LTPs) and nanometer optical measuring (NOM) like angular deflectometers, based on electronic autocollimator (AC) ELCOMAT-3000. The inherent systematic errors of the instrument's optical sensors set the principle limit to their measuring performance. Where autocollimator of a NOM-like profiler may be calibrated at a unique dedicated facility, this is for a particular configuration of distance, aperture size, and angular range that does not always match the exact use in a scanning measurement with the profiler. Here we discuss the developed methodology, experimental set-up, and numerical methods of transferring the calibration of one reference AC to the scanning AC of the Optical Surface Measuring System (OSMS), recently brought to operation at the ALS Xray Optics Laboratory. We show that precision calibration of the OSMS performed in three steps, allows us to provide high confidence and accuracy low-spatial-frequency metrology and not â€print into' measurements the inherent systematic error of tool in use. Here, with the examples of the OSMS measurements with a state-of-The-Art x-ray aspherical mirror, available from one of the most advanced vendors of X-ray optics, we demonstrate the high efficacy of the developed calibration procedure. The results of our work are important for obtaining high reliability data, needed for sophisticated numerical simulations of beamline performance and optimization of beamline usage of the optics. This work was supported by the U. S. Department of Energy under contract number DE-AC02-05CH11231.

47 OTHER INSTRUMENTATION↗

Temperature dependent structural, optical and hydrophobic properties of sputtered deposited HfO{sub 2} films

Hafnium oxide being high-k dielectric has been successfully utilized in electronic and optical applications. Being thermodynamically stable and having good mechanical strength, it can be used as a protective coating for outdoor HV insulators which are suffering from surface flashover problem due to contamination. In this paper, we are investigating the effect of substrate temperature on structural, optical and hydrophobic properties of hafnium oxide coating deposited over glass insulators by DC magnetron sputtering. X-ray diffraction is applied to determine the crystalline phase and crystallite size of the film. The morphology of the samples is examined using atomic force microscopy. The optical properties are studied using UV-vis-NIR spectrophotometer. The wettability of the film is investigated using contact angle meter. The thickness is measured using surface profilometer and verified through optical data. The relationship between substrate temperature with grain size, roughness, refractive index, and hydrophobicity is manifested. The maximum contact angle for HfO{sub 2} film was found to be 106° at 400°C.

36 MATERIALS SCIENCE↗

Characterization of electron microscopes with binary pseudo-random multilayer test samples

Verification of the reliability of metrology data from high quality X-ray optics requires that adequate methods for test and calibration of the instruments be developed. For such verification for optical surface profilometers in the spatial frequency domain, a modulation transfer function (MTF) calibration method based on binarypseudo-random (BPR) gratings and arrays has been suggested and and proven to be an effective calibration method for a number of interferometric microscopes, a phase shifting Fizeau interferometer, and a scatterometer. Here we describe the details of development of binarypseudo-random multilayer (BPRML) test samples suitable for characterization of scanning (SEM) and transmission (TEM) electron microscopes. We discuss the results of TEM measurements with the BPRML test samples fabricated from a WiSi{sub 2}/Si multilayer coating with pseudo-randomly distributed layers. In particular, we demonstrate that significant information about the metrological reliability of the TEM measurements can be extracted even when the fundamental frequency of the BPRML sample is smaller than the Nyquist frequency of the measurements. The measurements demonstrate a number of problems related to the interpretation of the SEM and TEM data. Note that similar BPRML testsamples can be used to characterize X-ray microscopes. Corresponding work with X-ray microscopes is in progress.

36 MATERIALS SCIENCE↗

Optical Imaging for Understanding of Thermal Barrier Coated Piston Engine Performance

Thermal barrier coatings (TBC) applied to pistons have been a recently renewed research topic in the field of internal combustion engines. Single cylinder testing of a conventional C15™ Tier 4 final pro-duction steel piston and a TBC coated piston showed that the Yttrium stabilized Zirconia (YSZ) TBC did not significantly alter engine performance, with the TBC piston having slower combustion rates and higher criteria emissions. For deeper understanding, research continued by studying 3D-piston sections optically in a constant pressure vessel using photodiodes, four high-speed cameras (natural luminosity, CH*, and OH*), and visualization of the flame from two orthogonal directions. Particle Im-aging Velocimetry (PIV) algorithms were adapted to perform Combustion Imaging Velocimetry (CIV) to aid in quantification of the observed visual combustion flow field differences. The optical work showed that the TBC piston flame development is slower, spatially different, with lower mixing energy for the TBC variant. Geometric profiles of engine pistons and optical vessel 3D-piston sections were measured using a Coordinate Measurement Machine (CMM), and surface roughness was measured with a stylus surface profilometer. CMM results showed that the TBC piston bowl had reasonable macroscopic accuracy, but the rim had a larger radius with less reentrancy. A discussion of the results and analyses in relation to future TBC effort and direction concludes the work.

33 ADVANCED PROPULSION SYSTEMS↗

Experimental Investigation of Turbine Vane Heat Transfer for Alternative Fuels

The focus of this program was to experimentally investigate advanced gas turbine cooling schemes and the effects of and factors that contribute to surface deposition from particulate matter found in coal syngas exhaust flows on turbine airfoil heat transfer and film cooling, as well as to characterize surface roughness and determine the effects of surface deposition on turbine components. The program was a comprehensive, multi-disciplinary collaborative effort between aero-thermal and materials faculty researchers and the Department of Energy, National Energy Technology Laboratory (NETL). The primary technical objectives of the program were to evaluate the effects of combustion of syngas fuels on heat transfer to turbine vanes and blades in land-based power generation gas turbine engines. The primary questions to be answered by this investigation were; What are the factors that contribute to particulate deposition on film cooled gas turbine components? An experimental program was performed in a high-temperature and pressure combustion rig at the DOE NETL; What is the effect of coal syngas combustion and surface deposition on turbine airfoil film cooling? Deposition of particulate matter from the combustion gases can block film cooling holes, decreasing the flow of the film coolant and the film cooling effectiveness; How does surface deposition from coal syngas combustion affect turbine surface roughness? Increased surface roughness can increase aerodynamic losses and result in decreased turbine hot section efficiency, increasing engine fuel consumption to maintain desired power output. Convective heat transfer is also greatly affected by the surface roughness of the airfoil surface; Is there any significant effect of surface deposition or erosion on integrity of turbine airfoil thermal barrier coatings (TBC) and do surface deposits react with the TBC in any way to decrease its thermal insulating capability? Spallation and erosion of TBC is a persistent problem in modern turbine engines; and What advancements in film cooling hole geometry and design can increase effectiveness of film cooling in turbines burning high-hydrogen coal syngas due to the higher heat loads and mass flow rates of the core flow? Experimental and numerical investigations of advanced cooling geometries that can improve resistance to surface deposition were performed. The answers to these questions were investigated through experimental measurements of turbine blade surface temperature and coolant coverage (via infrared camera images and thermocouples) and time-varying surface roughness in the NETL high-pressure combustion rig with accelerated, simulated surface deposition and advanced cooling hole concepts, coupled with detailed materials analysis and characterization using conventional methods of Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), X-Ray Diffraction (XRD), 3-D Surface Topography (using a 3-D stylus profilometer). Detailed surface temperatures and cooling effectiveness could not be measured due to issues with the NETL infrared camera system. In collaboration with faculty startup funding from the principal investigator, experimental and numerical investigations were performed of an advanced film cooling hole geometry, the anti-vortex hole (AVH), focusing on improving cooling effectiveness and decreasing the counter-rotating vortex of conventional cooling holes which can entrain mainstream particulate matter to the surface. The potential benefit of this program is in gaining a fundamental understanding of how the use of alternative fuels will effect the operation of modern gas turbine engines, providing valuable data for more effective cooling designs for future turbine systems utilizing alternative fuels.

10 SYNTHETIC FUELS↗

Environmental influences on autocollimator-based angle and form metrology

Deflectometric profilometers are indispensable tools for the precision form measurement of beam-shaping optics of synchrotrons and x-ray free electron lasers. They are used in metrology labs for x-ray optics worldwide and are crucial for providing measurement accuracy dictated by the form tolerances for modern state-of-the-art x-ray optics. Deflectometric profilometers use surface slope (angle) to assess form, and they utilize commercial autocollimators for the contactless slope measurement. In this contribution, we discuss the influences of environmental parameters, such as temperature and air pressure, including their gradients, on high-accuracy metrology with autocollimators in profilometers. They can cause substantial systematic errors in form measurement, especially in the case of large and strongly curved optical surfaces of high dynamic range. Relative angle and form measuring errors of the order of 10 -4 are to be expected. We characterize environmental influences by extended theoretical and experimental investigations and derive strategies for correcting them. Additionally, we report on the possibility to minimize the contributions of some errors by the application of sophisticated experimental arrangements and methods. We aim at approaching fundamental limits in autocollimator-based slope and form metrology.

47 OTHER INSTRUMENTATION↗

Explainable AI (XAI)-driven vibration sensing scheme for surface quality monitoring in a smart surface grinding process

Local Interpretable and Model-agnostic Explanation (LIME), an explainable artificial intelligence (XAI) approach is adapted to identify the globally important time-frequency bands for predicting average surface roughness (Ra) in a smart grinding process. The smart grinding setup consisted of a Supertech CNC precision surface grinding machine, instrumented with a Dytran piezoelectric accelerometer attached to the tailstock quill along the tangential direction (Y-axis). For every grinding pass, vibration signatures were captured, and the ground truth surface roughness values were recorded using a Mahr Marsurf M300C portable surface roughness profilometer. The roughness values ranged from 0.06 to 0.14 microns over the complete set of experiments. Time-frequency domain spectrogram frames were extracted for each of the vibration signals collected during the grinding process. Convolutional Neural Networks (CNNs) were modeled to predict the surface roughness based on these spectrogram frames and their image augmentations. The best CNN model was able to predict the roughness values with an overall R2-score of 0.95, training R2-score of 0.99, and testing R2-score of 0.81 with only 80 sets of vibration signals corresponding to 4 experiments with 20 trials each. Although the data size is not large enough to guarantee such performance metrics in real-world scenarios, one can extract statistically consistent explanations underlying the relationships these complex deep learning models capture. Further, the LIME methodology was implemented on the developed surface roughness CNN model to identify the important time-frequency bands (i.e., the superpixels of a spectrogram) influencing the predictions. Based on the identified important regions on the spectrogram frames, the corresponding frequency characteristics were determined that influence the surface roughness predictions. The important frequency range based on LIME results was approximately 11.7 to 19.1 kHz. The power of XAI was demonstrated by cutting down the sampling rate from 160 kHz to 30, 20, 10, and 5 kHz based on the important frequency range and considering Nyquist criteria. Separate CNN models were developed for these ranges by only extracting time-frequency contents below their corresponding Nyquist cut-offs. A proper data acquisition strategy is proposed by comparing the model performances to argue the selection of a sufficient sampling rate to capture the grinding process successfully and robustly.

42 ENGINEERING↗