Ronald Rogge National Research Council
Jim Theaker Atomic Energy Canada Ltd.
Camden Hubbard Oak Ridge National Laboratory
Rainer Schneider Hahn-Meitner-Institute
SS1: Qualifying New Materials I
Wednesday PM, December 03, 2008
Room 306 (Hynes)
9:30 AM - **SS1.1
The Critical Role of Metrology to Qualify New Materials for Space Applications.
Alexandre Cuenat 1 , Laurie Winkless 1 Show Abstract
1 , National Physical Laboratory, Teddington United Kingdom
The driving forces behind the materials development for space applications are numerous: improved performance, integrity and reliability of engineering systems, higher durability of products, higher efficiency, lower-energy consumption, light-weight, high-strength structures. To fulfil these requirements, there is a continuous need to develop new materials with specific functions: mechanical, thermal, optical electromagnetic, chemical and electronic. Nanomaterials represent an opportunity to meet these new specifications, but qualification of these new products will need accurate and reliable measuring and testing techniques. The National Physical Laboratory is at the forefront of the development of these measurement techniques to accreditate new nanomaterials for engineering applications. We will present the first results of a European- wide perspective on the potential use and the eventual barrier to nanomaterials applications for the space industry in the framework of a new ESA funded project. We will present our on-going work to define quantitatively how new nanomaterials can be used for space applications.
10:00 AM - **SS1.2
Regulating the use of New Materials in Containment Systems for Dangerous Goods.
Anton Erhard 1 , Th. Goedecke 1 , P. Blumel 1 , F. Otremba 1 Show Abstract
1 , Federal Insitute for Materials Research and Testing, Berlin Germany
10:30 AM - SS1.3
New Approaches to Systems Qualification: Long Term Ageing and Compatibility.
Julian Murphy 1 , Anthony Skinner 1 Show Abstract
1 , AWE, Reading, 0, United Kingdom
Volatile evolution from components within a system can lead to unexpected interactions resulting in reactions that have a detrimental effect upon the performance. This makes system qualification exceedingly difficult and time consuming. In the past the approach has been to first develop the individual components then to certify the system by looking for gross incompatibilities in simplified trials, where stacks of materials present in the system are sealed into vessels and subjected to an accelerated ageing regime. Such a procedure may fail to reproduce local environments found within real systems and subtleties associated with acceleration factors, which can vary significantly for different materials lead to difficulties in assigning an accurate lifetime equivalent age. Real time data can be obtained by monitoring systems in service and from breakdown and subsequent analysis of systems removed from service. Experience has shown that such data suffers from numerous drawbacks, it often has large scatter, is difficult to identify trends and can be of little value in adding additional assurance over that obtained from simplified trials.The presentation will outline a future strategy for systems qualification. This will require an assessment of long term ageing and systems compatibility during the initial stage of materials development programme. The rationale for performing trials to underwrite ageing and qualification that have increasing complexity to more accurately mimic the system as the design evolves, the materials and their specifications are decided and the manufacturing processes are developed will be discussed. Some of the approaches to experiment design and data analysis that enable confident qualification of the final system will be discussed and illustrated with some specific examples.
10:45 AM - SS1.4
Structural, Thermal and Rheological Studies on Newly Developed Polyesters Randomly Copolymerized with Poly(tetramethylene glycol) (PTMG).
Osamu Matsumoto 1 , Atsushi Hotta 1 Show Abstract
1 Graduate School of Science and Technology, Keio University, Yokohama Japan
Poly(cyclohexanedimethanol cyclohexanedicarboxlic acid) (PCC), a fairly newly synthesized polyester, has been studied and developed as an alternative material for rigid e.g. poly(vinyl chloroethylene) (PVC). Having a good experience of increasing both thermal stability and service temperature when applied to typical polymers, poly(tetramethylene glycol) (PTMG) was selected as a softening agent that randomly copolymerized into the PCC chains. Poly(ethylene terephthalate) (PET), the most widely used polyester, was also produced in order to investigate the effect of PTMG, which was compared with the properties of the newly developed random PCC-PTMG copolymers (PCC-r-PTMG). In this study, the crystalline structures, the thermal and the mechanical properties of PCC and PET containing different ratios of the random segment of PTMG were investigated by differential scanning calorimetery (DSC), polarized optical microscopy (POM) and tensile tester.It was found that the crystallization rate of pure PCC was significantly slow, whereas for PCC-r-PTMG, PTMG accelerated the crystallization rate with increasing PTMG, and the sample with 25wt% of PTMG had the fastest crystallization rate in all PCC-r-PTMG samples. Here, the PTMG acted as an accelerator, simultaneously depressing the movement of PCC molecular chains. The morphology of the crystal was predominantly spherulite observed by POM, while the spherulite became increasingly incomplete as PTMG was added into the PCC. The tensile test results showed that the fracture strain increased and the Young modulus decreased with increasing PTMG, indicating that the mechanical properties of PCC-r-PTMG were significantly affected by the content of PTMG. Moreover, the elastic recovery test indicated that the ability of PTMG as a softening agent was highly demonstrated at 20wt% of PTMG. The results of PCC-r-PTMG were compared with those of PET-r-PTMG and it was found that there were optimum values of PTMG for the crystallization rate on both samples. Additionally, the results of the elastic recovery test indicated that the softening effects observed for PCC-r-PTMG were more pronounced than those observed for PET-r-PTMG. From all these results, it was concluded that PCC was highly promising polyester to be used as an alternative material for PVC.
11:45 AM - SS1.6
Structural Transformation and Mechanical Properties of Cold Sprayed Copper and Nickel Coatings after Annealing.
Yu Zou 1 , Ahmad Rezaeian 1 , Jerzy Szpunar 1 , Eric Irissou 2 , Steve Yue 1 Show Abstract
1 Metals and Materials Engineering, McGill University, Montreal, Quebec, Canada, 2 Industrial Materials Institute(IMI), National Research Council Canada(NRC) , Boucherville, Quebec, Canada
Pure copper and nickel coatings were fabricated by Cold Spray (CS) manufacturing process. The as-sprayed coatings were annealed in air for one hour at various temperatures from 100°C up to 600°C. Structural transformation was investigated by Electron Backscattering Diffraction (EBSD) using a FEG-SEM to determine the state of stress, grain size distribution and texture of both the as-sprayed and air annealed coatings. Micro hardness transformation was recorded as function of annealing temperature. The results showed that recrystallization occurred in Copper after annealing at temperatures higher than 250 °C and in nickel coatings at 400 °C, but no obvious grain growth across the thickness of sprayed coatings was observed. The data of Kernel Average Misorientation (KAM), that represents the dislocation density distribution, demonstrated that the particles were heavily deformed around the edges, but not deformed in the center. The residual stress and the dislocation density in the deformed areas decreased during the annealing process. Only weak texture was observed after various stages of the annealing process. The ductility and formability were significantly improved after annealing.
SS2: In-Room Poster Session I
Wednesday PM, December 03, 2008
Room 306 (Hynes)
12:00 PM - SS2.1
Enzymatic Polymerization of Quercetin and Modeling Studies for Structural Elucidation.
Adam Trotta 2 , Stephen Fossey 1 , Subhalakshmi Nagarajan 2 , Ramaswamy Nagarajan 4 , Lynne Samuelson 1 , Jayant Kumar 3 , Ferdinando Bruno 1 Show Abstract
2 Chemistry, UMASS Lowell, Lowell, Massachusetts, United States, 1 Material Science, US Army Natick Lab, Natick, Massachusetts, United States, 4 Plastics Engineering and Center of Green Chemistry, UMASS Lowell, Lowell, Massachusetts, United States, 3 Physics, UMASS Lowell, Lowell, Massachusetts, United States
Quercetin is a flavonol found in fruits, onions and wine. Recently, quercetin has been extensively investigated for its antioxidant behavior in food such as poultry and fish. However, increasing the thermal stability and the antioxidant potency of this flavonol would be beneficial to the food industry. We utilized Horseradish Peroxidase (HRP), a phytochemical enzyme, to polymerize quercetin in a water/ethanol mixture. This unique, one pot procedure has provided a method to synthesize polyquercetin under mild conditions. The final polymer is soluble in a water/ethanol mixture. One of the purposes of this work is to characterize the proposed polyquercetin by various instrumental techniques. Using UV-Vis and FTIR, MS-MS we deduced certain aspects of the structure. Moreover, experimental work was teamed with modeling. Density functional theory calculations show that the UV-Vis spectra of polyquercetin are blue shifted relative to those of quercetin monomer. This was confirmed by the experimental measurements. This novel thermally stable polymer, synthesized using Green Chemistry, can be of interest in the highly regulated food industry.
12:00 PM - SS2.2
Nanometrology Proficiency Test of International Laboratory Comparison on One Dimensional Grating Pitch Measurement.
Chien-Ying Su 1 2 , Y. Lin 1 2 , S. Pai 1 , P. Chen 1 , N. Chu 1 , C. Yang 1 , J. Kao 1 Show Abstract
1 , Instrument Technology Research Center, National Applied Research Laboratories, Hsinchu City Taiwan, 2 , National Chiao Tung University, Hsinchu Taiwan
The aim of this study is to realize the ability of measuring 1D fine pitch as nanometrology standard. Participants are from government and industry labs, and our laboratory has been invited to participate in this activity. The scale of the pitch standard have been chosen to be suitable for both diffractometers and scanning probe microscopes (SPM). The measurement procedure takes into consideration the previous experience gained in the Consultative Committee for Length (CCL) Nano4 Supplementary Comparison. Our measurement results show conformity according to ISO/IEC Guide 43, and the average deviation is less than 0.2%.
12:00 PM - SS2.3
Effect of Rinkalore Mixture on the Flotation of Mupine Oxidised Ores, South DRCongo.
Tshilombo Ghislain 1 Show Abstract
1 , Council for Scientific and Industrial Research, Pretoria South Africa
In this study, flotation of oxidised ores rich in copper and cobalt from Mupine deposit in the Democratic Republic of Congo had been investigated. This ore contains 4.85% copper, 0.16% cobalt. The recovery of copper and cobalt was performed using flotation to increase the concentration of copper and cobalt. Flotation of the oxidized ore was performed with fatty acid type Rinkalore. Copper and cobalt present in the ore were concentrated with optimal doses of sodium silicate, Rinkalore mixture of 500 g/t, 1500 g/t respectively and optimum tall oil and pH of 23% and 9.5 respectively. The influence of Rinkalore Bioex, Rinkalore Booster Q, pH and sodium silicate on optimum operating conditions were studied. Improved performance of operating conditions was obtained with the mixture of reagents Rinkalores 10 and Booster Q. Primary feed titrating 8.70% copper and 0.31% cobalt respectively had a recovery yield of 53% and 34% respectively, and rougher concentrate titrating 8.13% copper and 0.33 % Cobalt respectively had a recovery yield of 97% and 70% respectively.
12:00 PM - SS2.4
Improved Specification of a Polyurethane Adhesive Increasing Confidence in Re-qualification After Changes.
Julian Murphy 1 , Laura Pilon 1 Show Abstract
1 , AWE, Reading, 0, United Kingdom
Historically, materials developed at AWE have used commercially supplied material, which are often given loose specifications by their suppliers. The specifications used at AWE to determine the suitability of a material for use were defined by both the suppliers specification and the requirements of the manufacturing processes. These process requirements may not be affected by changes in the properties of the materials used in them, but small changes in a precursor properties can have a large effect upon the important, in-service, properties of the final material. In the case of a polyurethane adhesive developed from a commercially supplied polyester precursor, significant changes in the nature of the polyester between batches have been identified. Such changes have led to difficulties in sustaining the manufacturing process, since the properties have drifted outside the specification for this material. More accurate measurement of the important properties of the polyester (by SEC and NMR) have led to an increased understanding of the material. In particular, correct determination of the molecular weight, and branched nature of the polyester allows for increased accuracy in specifying the mechanical properties of the end material. Increased confidence in the reproducibility of materials then leads to an easier and quicker qualification process.
12:00 PM - SS2.5
Development of Metallic Materials.
Andrew Wallwork 1 , Tim Cartwright 1 , Michael Cox 1 , Anthony Ward 1 , Bernard Haley 1 , Francis Davis 1 Show Abstract
1 Material Science Research Division, AWE, Reading United Kingdom
This poster will provide an overview of research and development work ongoing at AWE to assess a wide variety of metallic materials. This research work incorporates material identification, manufacture and assessment. The latter requires extensive material characterisation using a wide range of experimental techniques including optical metallography, X-Ray Diffraction (XRD), Electron Backscattered Diffraction (EBSD), Transmission Electron Microscopy (TEM) and where appropriate Neutron Diffraction. Extensive mechanical testing is also completed, notably obtaining compressive, tensile and fracture properties over a wide strain rate and temperature range. Finally, where appropriate, ageing experiments are undertaken to assess chemical compatibility as well as mechanical/chemical affects, notably stress corrosion cracking. The output from the research work can then be used to develop continuum models that predict material behaviour with age. This information (experimental and computational) can then be employed to underwrite metallic materials with high levels of assurance.
12:00 PM - SS2.6
Quick Synthesis of Large Area Diamond like Carbon Thin Films by Dielectric Barrier Discharge under Atmospheric Pressure.
Xinpeng Wang 1 , Xianping Feng 1 Show Abstract
1 Physics, University of Puerto Rico, San Juan, Puerto Rico, United States
Dielectric barrier discharge has been employed to yield diamond like carbon thin films under atmospheric pressure. Quick syntheses have been achieved to obtain such thin films. The thickness of thin film was around 200 nm under 10 minute’s deposition. Different types of methane-hydrogen-argon contents were adopted to synthesize large area diamond like carbon films. It was found that deposition only at argon concentration equal or less 75% yielded typical diamond like carbon film. Too high content argon content during deposition gave rise to graphite type of the thin films. Such results have been confirmed based on the XPS, FTIR and Raman spectra and their hardness measurements. In particular, when lowering The lower argon concentration from 75% to 0, the intensity ratio of G band versus D band increases from 1.6 to 2.1. On the other hand, the plasma morphology was not uniform when lowering the argon concentration, which resulted in much higher roughness of thin film. Due to both advantage and disadvantage, the influences of argon concentration on diamond like carbon thin films hardness, elasticity and roughness have been discussed, and an optimized methane-hydrogen-argon content was found.
SS3: Qualifying New Materials II
Wednesday PM, December 03, 2008
Room 306 (Hynes)
2:30 PM - **SS3.1
Innovation in Quality Control using Validated Non-destructive Testing Methods in Accordance with International Standards for Flexible Lab Accreditation.
Bernd Valeske 1 , S. Kraus 1 Show Abstract
1 , Fraunhofer Institute for non-destructive testing (IZFP), Saarbrucken Germany
3:00 PM - **SS3.2
Development of Simplified Organic Materials to Enable Easier Qualification.
Julian Murphy 1 , Anthony Swain 1 , Mogon Patel 1 Show Abstract
1 MSRD, AWE, Reading United Kingdom
3:30 PM - SS3.3
Multi-Material Accelerated Ageing Experiments: Experimental Challenges and Diagnostic Development.
Scott McCulloch 1 Show Abstract
1 , Systems Monitoring AWE, Reading United Kingdom
The qualification of materials for use in certain aerospace and nuclear environments has a number of challenges, which can include demonstrating “fitness-for-service” over extended, typically decade long, time-scales. This may further be complicated by the requirement to meet the stringent demands of governmental agencies, which require absolute confidence that the materials system will remain within specification throughout its service life. The validation of materials over such extended time-scales represents a significant materials development challenge, and provides an opportunity for the introduction of both conventional and unique experimental techniques to assist in the characterisation of the overall materials system. In this paper we describe a multi-material experiment which has been subjected to an artificial ageing regime, and in which the pressure of the gaseous head-space surrounding the materials is monitored and the final gas-composition analysed. Experimental challenges resulting from the complex nature of the materials involved will be highlighted. In order to enhance the fidelity of the gas-composition information, in-situ diagnostics that probe gas-composition have been used. The development of these diagnostics will be described, which includes novel optical fibre-based spectroscopic techniques that can be been applied to materials environments in which there is limited free volume and no direct optical measurement path.
3:45 PM - SS3.4
Temperature Effect on Alkanes Evaporation Rates: Proper Lubricant Selection.
Alex Volinsky 1 , Nathaniel Waldstein 1 Show Abstract
1 Mechanical Engineering, University of South Florida, Tampa, Florida, United States
Miniature mechanisms require small amounts of lubrication to reduce friction. Lubricants can evaporate over time at elevated temperatures, as the evaporation rate has exponential temperature dependence described by the Arrhenius equation. This paper presents the methodology of measuring alkanes evaporation rates at varying temperatures and discusses proper lubricant selection for applications in several industries. The evaporation rates of alkanes were measured in an attempt to predict oil evaporation rates based on its chemical composition.
4:30 PM - SS3.5
Structural, Optical and Electrical Properties of InGaN Sputtered Thin Films.
Mohammad Ebdah 1 , D. Hoy 1 , J. Vaughn 1 , M. Kordesch 1 Show Abstract
1 Department of Physics and Astronomy, Ohio University, Athens, Ohio, United States
Structural, Optical and Electrical Properties of InGaN Sputtered Thin FilmsM. A. Ebdah, D. R. Hoy, J. M. Vaughn, M.E. KordeschDepartment of Physics and Astronomy, Ohio University, Athens, OH 45701.InGaN thin films have been recently of great considerations in high efficiency photovoltaics and radio frequency technologies. The incorporation of InGaN in device applications and low cost high temperature electronics has been well established in industrial applications. In this work, InGaN films were successfully fabricated using rf sputtering technique with a sputtering target of polycrystalline In and Ga species under the flow of Nitrogen. Films were deposited on Si and glass substrates, with the ratio of In to Ga being varied from 0 to 1 in the alloy. Growth under different sputtering conditions has been examined, such as different temperatures, pressures, and substrate-target distances. The corresponding obtained structures have been studied using the x-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques. The compositions have been varified by means of energy dispersive x-rays (EDX) spectroscopy and Rutherford back scattering (RBS). Multiple crystallographic phases have been investigated upon growth at different temperatures, and the existence of Gallium Nitride (GaN) and Indium Nitride (InN) phases was investigated. Hall effect measurements were made in 0.55 T magnetic field for characterizing the electrical resistivity at room temperature and 77 K, the free carrier concentration, and mobility. The optical bandgap and optical properties were studied by spectrophotometric and spectroscopic ellipsometric (SE) techniques.
4:45 PM - SS3.6
Annealing Phenomena in Electrodeposited Ni/Invar Bimetals.
Jeong Ho Seo 1 , Myung Jae Lee 1 , Yong Bum Park 1 Show Abstract
1 Materials Science, Sunchon National University, Suncheon, Jeonnam, Korea (the Republic of)
5:00 PM - SS3.7
Phosphation of TiO2 at High Temperature to Perform High Photocatalytic Activity.
Sue-min Chang 1 , Chieh-yao Hou 1 , Pin-shin Sung 1 Show Abstract
1 Institute of Environmental Enginnering, National Chiao Tung Univesrity, Hsinchu Taiwan
Phosphated TiO2 has been proved exhibiting high photoacatalytic activity because of high surface acidity and extended charge life time. In this study, we firstly demonstrate that phoshation of TiO2 at high temperature greatly improves it photocatalytic activity rather than at low temperature. Phosphation process undergoes calcination of TOPO capped-TiO2 anatse nanocrystals. Calcination completely burns out the organic part of the TOPO and leaves phosphrous ions incorporated into TiO2 surface lattice above 550 °C. Hydroxylated surface and PO43- units are initially formed at the surface of the TiO2. However, thermal induced dehydroxylation takes place at 750 °C, and polyphosphate moieties are introduced as the temperature rise to 950 °C. Phosphation maintains the metastability of anatase form and inhibits the growth of crystallite sizes (5.2-5.4 nm) against heating till 930 °C. Calcination transforms the anatse to rutile phase and increases the crystallites sizes to 1.81×10-2 nm at 950 °C. Meanwhile, the specific surface area of the phosphated TiO2 dramatically declines from 159 to 0.81 m2/g. Photocatalytic activity of the phosphated TiO2 is examined by decoloration of rhodamine B under illumination of UV light at 305 nm. The specific rate constant of the phosphated TiO2 at 950 °C is 3.0 × 10-2 g/min/m2, which is 2.5 and 50 times higher than that of P25 (1.2 × 10-2 g/min/m2) and the phosphated TiO2 at 550 °C (6.3 × 10-4 g/min/m2), respectively. The formation of polyphosphate species governs the high photocatalytic activity of the phophated TiO2 calcined at high temperature.