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At least 667 records · Page 37

NDE Technology Engineering Program for Hanford DST Non-Visual Volumetric Inspection Technology: Phase II RAVIS Radiation Tolerance Test Report

This test report provides the results of radiation tolerance robustness testing that was performed on samples of robotic components and an ultrasonic guided wave air-slot sensor that represent components/sub-systems of the Robotic Air-slot Volumetric Inspection System (RAVIS) that has been engineered for volumetric inspection of Hanford tank bottom plates via under-tank refractory pad air-slots. The specific components tested for 1) functionality during active irradiation and 2) tolerance to cumulative radiation dose (until failure or upon reaching a cumulative dose test limit) were: • four samples each of a printed circuit board (PCB) and direct current (DC) motor, which are robotic components, and • 26 ultrasonic piezoelectric elements (samples) inside an air-slot sensor. The robotic components are part of the RAVIS air-slot inspection crawler drive control system that is responsible for remote communication with and actuation of the air-slot inspection crawler. The failure of either of these components during under-tank deployment would require manual retrieval via the crawler’s tether, which risks damage to the robot/refractory/tank. Preemptive replacement of the components at appropriately conservative dose/time intervals informed by failure dose would reduce the likelihood of under-tank failure. The components were included in radiation tolerance testing to quantify their failure doses to inform replacement intervals. The air-slot sensor is responsible for collecting ultrasonic inspection data (scan images) for the tank bottom plates during under-tank deployment. Compromised signal quality due to elevated noise levels caused by gamma radiation would compromise inspection performance. The air-slot sensor was included in radiation tolerance testing to quantify the impact of active irradiation on sensor signal quality. The irradiation and in-situ functional tests of the PCBs, DC motors and air-slot sensor took place in June and July 2020 at the Pacific Northwest National Laboratory. Testing was performed at a gamma dose rate near 300 rad/hr., which, in the absence of under-tank dose rate data, has been conservatively estimated to be the upper-bound dose rate beneath the primary tanks at Hanford. Irradiation took place at elevated temperatures of 150-200°F to determine failure doses that reflect the compounding effects of gamma radiation and heat. The test results revealed: • The DC motors can tolerate being actively irradiated at the high dose rate at 200°F and can tolerate a cumulative dose of 300,000 rad, that which would be incurred after 5 years of service at the 300 rad/hr dose rate. The component therefore meets minimum and preferred radiation tolerance and lifecycle requirements for robotic components. • The air-slot sensor can tolerate being actively irradiated at the high dose rate at 150°F and can tolerate a cumulative dose of 60,000 rad, that which would be incurred after 1 year of service at the 300 rad/hr dose rate. The sensor therefore meets minimum radiation tolerance and lifecycle requirements. • The PCB can tolerate being actively irradiated at the high dose rate, but can only tolerate a cumulative dose of 19,000 rad at 150-200°F. The PCB does not meet minimum radiation tolerance and lifecycle requirements; however, because the component is considered replaceable, it can be replaced before a cumulative dose of 19,000 rad is reached, determined through either monitoring with a dosimeter or scheduled time intervals that are calculated based on conservative estimates of under-tank dose rates.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

SkyMine Carbon Mineralization Pilot Project

This Topical Report addresses accomplishments achieved during Phase 2b of the SkyMine® Carbon Mineralization Pilot Project. The primary objectives of this project are to design, construct, and operate a system to capture CO2 from a slipstream of flue gas from a commercial coal-fired cement kiln, convert that CO2 to products having commercial value (i.e., beneficial use), show the economic viability of the CO2 capture and conversion process, and thereby advance the technology to the point of readiness for commercial scale demonstration and deployment. The overall process is carbon negative, resulting in mineralization of CO2 that would otherwise be released into the atmosphere. The project will also substantiate market opportunities for the technology by sales of chemicals into existing markets, and identify opportunities to improve technology performance and reduce costs at the commercial scale. The project is being conducted in two phases. The primary objectives of Phase 1 were to evaluate proven SkyMine® process chemistry for commercial pilot-scale operation and complete the preliminary design for the pilot plant to be built and operated in Phase 2, complete a NEPA evaluation, and develop a comprehensive carbon life cycle analysis. The objective of Phase 2b was to build the pilot plant to be operated and tested in Phase 2c.

Christenson, Norm↗

EBS Task Force: Task 9/FEBEX Modeling Final Report: Thermo-Hydrological Modeling with PFLOTRAN

This report outlines Sandia National Laboratories modeling studies applied to Stage 1 and Stage 2 of the Full-scale Engineered Barriers Experiment in Crystalline Host Rock (FEBEX) in situ test for the SKB EBS Task Force Task 9. The FEBEX test was a full-scale test conducted over ~18 years at the Grimsel, Switzerland Underground Research Laboratory (URL) managed by NAGRA. It involved emplacing simulated waste packages, in the form of welded cylindrical heaters, inside a tunnel in crystalline granitic rock and surrounded by a bentonite barrier and cement plug. Sensors emplaced within the bentonite monitored the wetting-up, heating, and drying out of the bentonite barrier, and the large resulting data set provides an excellent opportunity for validation of multiphysics Thermal-Hydrological (TH), Thermal-Hydrologic-Chemical (THC), and Thermal-Hydrological-Mechanical (THM) modeling approaches for underground nuclear waste storage and the performance of engineered bentonite barriers. The present status of the EBS Task Force is finalizing Task 9, which follows years of modeling studies of the FEBEX test, by many notable modeling teams (Gens et al., 2009; Sanchez et al. 2010; 2012; Samper et al., 2018). These modeling studies generally use two-dimensional axisymmetric meshes, ignoring threedimensional effects, gravity and asymmetric wetting and dry out of the bentonite engineered barrier. This study investigates these effects with use of the PFLOTRAN THC code with massively parallel computational methods in modeling FEBEX Stage 1 and Stage 2 results. The PFLOTRAN numerical code is an open source, state-of-the-art, massively parallel subsurface flow and reactive transport code operating in a high-performance computing environment (Hammond et al., 2014). Section 2 describes the applied partial differential equations describing mass, momentum and energy balance used in this study, considerations derived by assuming phase equilibrium between gas and liquid phases, constitutive equations for granite, cement plug, and bentonite domains, and specific approaches for use inthe PFLOTRAN code. Section 3 describes the geometry, meshing, and model set-up. Section 4 describes modeling results, Section 5 compares modeling results to field testing data, and Section 6 gives conclusions. The Appendix provides detailed information required by the EBSTask Force for final reporting.

42 ENGINEERING↗

Systematic study on the influence of the morphology of α-MoO{sub 3} in the selective oxidation of propylene

A variety of morphologically different α-MoO{sub 3} samples were prepared by hydrothermal synthesis and applied in the selective oxidation of propylene. Their catalytic performance was compared to α-MoO{sub 3} prepared by flame spray pyrolysis (FSP) and a classical synthesis route. Hydrothermal synthesis from ammonium heptamolybdate (AHM) and nitric acid at pH 1–2 led to ammonium containing molybdenum oxide phases that were completely transformed into α-MoO{sub 3} after calcination at 550 °C. A one-step synthesis of α-MoO{sub 3} rods was possible starting from MoO{sub 3}·2H{sub 2}O with acetic acid or nitric acid and from AHM with nitric acid at 180 °C. Particularly, if nitric acid was used during synthesis, the rod-like morphology of the samples could be stabilized during calcination at 550 °C and the following catalytic activity tests, which was beneficial for the catalytic performance in propylene oxidation. Characterization studies using X-ray diffraction (XRD), scanning electron microscopy (SEM) and Raman spectroscopy showed that those samples, which retained their rod-like morphology during the activity tests, yielded the highest propylene conversion. - Graphical abstract: Hydrothermal synthesis from MoO{sub 3}·2H{sub 2}O in the presence of HNO{sub 3} led to rod-shaped particles which mainly expose (1 0 0) facets which are the most active surfaces. - Highlights: • Hydrothermal synthesis of MoO3 resulted in either rod or slab shaped particles depending on pH. • At pH<0 rods stable towards calcination and catalytic activity testing were formed. • Rod shaped particles had significantly higher activity than slab shaped ones. • The rod shaped particles mainly expose the (1 0 0) facets which are the most active surfaces. • Total surface area is not main determining factor for catalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Observation of Unconventional Dynamics of Domain Walls in Uniaxial Ferroelectric Lead Germanate

Application of scanning probe microscopy techniques such as piezoresponse force microscopy (PFM) opens the possibility to re-visit the ferroelectrics previously studied by the macroscopic electrical testing methods and establish a link between their local nanoscale characteristics and integral response. It is reported that the nanoscale PFM studies and phase-field modeling of the static and dynamic behavior of the domain structure in the well-known ferroelectric material lead germanate Pb 5 Ge 3 O 11 . Here, several unusual phenomena are revealed: 1) domain formation during the paraelectric-to-ferroelectric phase transition, which exhibits an atypical cooling rate dependence; 2) unexpected electrically induced formation of the oblate domains due to the preferential domain walls motion in the directions perpendicular to the polar axis, contrary to the typical domain growth behavior observed so far; 3) absence of the bound charges at the 180 degrees head-to-head (H-H) and tail-totail (T-T) domain walls, which typically exhibit a significant charge density in other ferroelectrics due to the polarization discontinuity. This strikingly different behavior is rationalized by the phase field modeling of the dynamics of uncharged H-H and T-T domain walls. The results provide a new insight into the emergent physics of the ferroelectric domain boundaries, revealing unusual properties not exhibited by conventional Ising-type walls.

36 MATERIALS SCIENCE↗

Design of interferometer system for Keda Torus eXperiment using terahertz solid-state diode sources

A solid-state source based terahertz (THz) interferometer diagnostic system has been designed and characterized for the Keda Torus eXperiment (KTX). The THz interferometer utilizes the planar diodes based frequency multiplier (X48) to provide the probing beam at fixed frequency 0.650 THz, and local oscillator is provided by an independent solid-state diode source with tunable frequency (0.650 THz +/− 10 MHz). Both solid-state sources have approximately 1 mW power. The planar-diode mixers optimized for high sensitivity, ∼750 mV/mW, are used in the heterodyne detection system, which permits multichannel interferometer on KTX with a low phase noise. A sensitivity of {sub min} = 4.5 × 10{sup 16} m{sup −2} and a temporal resolution of 0.2 μs have been achieved during the initial bench test.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Understanding Environmental Barrier Coating Lifetimes and Performance for Industrial Gas Turbines

Hydrogen or hydrogen blend fuels are expected to replace natural gas in land-based industrial gas turbines (IGTs) to support a greener power economy. Silicon carbide (SiC) base ceramic matrix composites (CMCs) are considered for replacement of Ni-based superalloys to facilitate future efficiency improvements. SiC CMCs require environmental barrier coatings (EBCs) to mitigate volatilization from high-temperature steam, thus making the EBC lifetime critical information for identifying CMC component lifetimes. Here, the goal of this project is to determine the maximum bond coating temperature underneath the EBC for achieving an IGT component lifetime goal of 25,000 h, which is far greater than current CMC component lifetime requirements for aeroturbine applications. To provide data for the lifetime model, laboratory testing used atmospheric plasma-sprayed rare-earth silicate EBCs on monolithic SiC substrates with an intermediate Si bond coating. Specimens exposed to 1-h thermal cycles in flowing air–steam environments and reaction kinetics were assessed from 700 °C to 1350 °C by measuring the thickness of the thermally grown silica scales. The silica growth and phase transformation appear critical in predicting EBC lifetime and several strategies have been explored to reduce the oxide growth rate and improve EBC durability at elevated temperatures. Advanced characterization using Raman spectroscopy has helped clarify this system.

08 HYDROGEN↗

PIP-II Project Overview and Status

The Proton Improvement Plan II (PIP-II) project is an essential upgrade to Fermilab’s particle accelerator complex to enable the world’s most intense neutrino beam for LBNF/DUNE and a broad particle physics program for many decades to come. PIP-II will deliver 1.2 MW of proton beam power from the Main Injector, upgradeable to multi-MW capability. The central element of PIP-II is an 800 MeV superconducting radio frequency (SRF) linac, which comprises a room temperature front end followed by an SRF section. The SRF section consists of five different flavors of cavities/cryomodules, including Half Wave Resonators (HWR), Single Spoke and elliptical resonators operating at, or above, state-of-the-art parameters. The first two PIP-II cryomodules, Half Wave Resonator (HWR) and Single Spoke Resonator 1 (SSR1) were installed in the PIP-II Injector Test facility (PIP2IT) and have accelerated beam to above 17 MeV. PIP-II is the first U.S. accelerator project that will be constructed with significant contributions from international partners, including India, Italy, France, United Kingdom and Poland. The project was baselined in April 2022, and the construction phase is underway.

43 PARTICLE ACCELERATORS↗

Developing quantitative capabilities for a scanning microwave impedance microscope

Currently no instrument exists to quantitatively measure electrical properties (dielectric constant and conductivity) on sub-micron regions, a capability of extreme importance to measure the functioning of sub-micron structures and devices. In particular, such electrical measurements could support the development and manufacture of advanced energy related materials used in technologies such as photovoltaic cells, fuel cells and advanced batteries, thereby increasing performance and/or lowering production costs. The goal of this project is to develop microwave imaging add-on modules and probes capable of quantitatively measuring the electrical properties of small regions of a material using microwaves. These modules for scanning probe microscopes, such as atomic force microscopes, make use of the near-field interaction between the exciting microwaves and a material and can resolve regions 10 nanometers in size (less than a million atoms) with little perturbation of the material. In Phase 1 commercial probes and modified hardware were used to establish the feasibility of using microwave imaging systems to quantify local permittivity and conductivity. Repeatable measurements that vary in a systematic way with electrical parameters were obtained from a variety of samples. In Phase 2 research prototypes of the needed hardware and probes were developed and their performance against test structures and real-world samples was demonstrated. Result of this research project include demonstration of quantification of both permittivity and doping level at precisions up to 10% using multiple technical approaches. The level of performance and ease of use meets market expectations and the technology and protocols researched under this grant are currently being commercialized. Quantitative capabilities of this sort will provide a key capability to energy related technologies, and to a wide variety of semiconductor, biological, and materials science applications. Applications include both materials research in academic and industrial labs, as well as manufacturing applications. In a manufacturing environment the quantitative measurement and imaging capabilities could be used both as metrology for process control and as a tool for failure analysis and yield improvement.

36 MATERIALS SCIENCE↗

Long-term Dynamical Stability in the Outer Solar System. I. The Regular and Chaotic Evolution of the 34 Largest Trans-Neptunian Objects

We carried out an extensive analysis of the stability of the outer solar system, making use of the frequency analysis technique over short-term integrations of nearly 100,000 test particles, as well as a statistical analysis of 200 1 Gyr long numerical simulations, which consider the mutual perturbations of the giant planets and the 34 largest trans-Neptunian objects (we have called all 34 objects “dwarf planets,” DPs, even if probably only the largest of them are true DPs). From the frequency analysis, we produced statistical diffusion maps for a wide region of the a–e phase-space plane; we also present the average diffusion time for orbits as a function of perihelion. We later turned our attention to the 34 DPs, making an individualized analysis for each of them and producing a first approximation of their future stability. From the 200 distinct realizations of the orbital evolution of the 34 DPs, we classified the sample into three categories, including 17 stable, 11 unstable, and 6 resonant objects; we also found that, statistically, two objects from the sample will leave the trans-Neptunian region within the next gigayear, most likely being ejected from the solar system, but with a nonnegligible probability of going inside the orbit of Neptune, either to collide with a giant planet or even falling to the inner solar system, where our simulations are no longer able to resolve their continuous evolution.

79 ASTRONOMY AND ASTROPHYSICS↗

Improvement of the fracture toughness of hydroxyapatite (HAp) by incorporation of carboxyl functionalized single walled carbon nanotubes (CfSWCNTs) and nylon

The potential of improving the fracture toughness of synthetic hydroxyapatite (HAp) by incorporating carboxyl functionalized single walled carbon nanotubes (CfSWCNTs) and polymerized ε-caprolactam (nylon) was researched. A series of HAp samples with CfSWCNTs concentrations varying from 0 to 1.5 wt.%, without, and with nylon addition was prepared. X-ray diffraction (XRD), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM) were used to characterize the samples. The three point bending test was applied to measure the fracture toughness of the composites. A reproducible value of 3.6 ± 0.3 MPa.√m was found for samples containing 1 wt.% CfSWCNTs and nylon. This value is in the range of the cortical bone fracture toughness. Lastly, the increase of the CfSWCNTs content results to decrease of the fracture toughness, and formation of secondary phases.

36 MATERIALS SCIENCE↗

In situ characterization of two unknown ultrashort laser pulses using four-wave mixing in gas

Accurate characterization of two ultrashort laser pulses is of great interest in many ultrafast pump-probe experiments. We demonstrate a method based on four-wave mixing (FWM) in a gas which could be easily implemented into many existing pump-probe setups with minimal modifications for accurate, in situ characterization of both unknown pulses. This technique is tested on pairs of unknown pulses at wavelengths of 400/800 nm, and 266/400 nm. We measured the spectrogram of the pulse generated through FWM of the two unknown pulses by scanning the delay between two unknown pulses. The retrieval algorithm converges to accurately predict the intensity and the phase profiles of both unknown pulses with a trace error of < 1% and the accuracy is verified using an independent pulse characterization device.

Nambu, Noa (ORCID:0000000197303400)↗

Storage Field Development Plan: One Earth Energy

This Storage Field Development plan presents the Storage Complex characterization results, construction, monitoring, and operational plans, and costs associated with the proposed One Earth Sequestration Carbon Capture and Storage (OES-CCS) site in McLean County, Illinois, near Gibson City. The proposed storage complex, known as the Mt. Simon Storage Complex, comprises the Cambrian Mt. Simon Sandstone reservoir and the primary seal, the Cambrian Eau Claire Formation. The lowermost Underground Source of Drinking Water (USDW) identified for the site is the Ordovician St. Peter Sandstone. Geologic characterization of the Mt. Simon Storage Complex at the OES-CCS site was performed by the Illinois Storage Corridor CarbonSAFE Phase III project, which also prepared and submitted three UIC Class VI applications to construct three injection wells; the permit applications were submitted and are in the federal EPA review process. A characterization well, OEE #1, was drilled to collect site-specific data. These data were analyzed and used to develop the UIC Class VI applications. The OEE #1 well will be converted to an in-zone monitoring (IZM) well for the injection phase. The proposed buildout for the OES-CCS site includes (1) three injection wells (OES #1, OES #2, and OES #3), (2) two IZM wells, (3) two above confining zone (ACZ) monitoring wells, one of which will be used to monitor the lowermost USDW, (4) capture and compression facilities, and (5) transportation facilities, i.e., pipelines. A pre-operational testing program was proposed in the Class VI permit application and will be employed at the site pending approval. Additional pre-injection (baseline), syn-injection, and post-injection monitoring and site care procedures will be followed by OES to ensure that injection activities are protective of human health and the environment. Injection is scheduled to begin in 2025, distributed across the three injection wells in accordance with the permit operating conditions. One Earth Sequestration intends to inject up to 90 million tonnes of CO 2 over a period of approximately 20 years. Injection will begin at approximately 0.5 million tonnes of CO 2 annually and ramp up to a maximum of 4.5 million tonnes annually. Daily injection rates are expected to range from 1,400 to 1,500 tonnes per day initially and reach a maximum of approximately 4,225 tonnes per day, depending on site geology and injectivity at each injection well location, and CO 2 availability. The costs associated with the OES-CCS project include pre-operational costs (e. g. additional seismic data acquisition and well drilling), capture and transportation facility and equipment costs, predicted field operating expenditures (OpEx), and decommissioning and post-injection site care (PISC) costs. The risks associated with project activities, such as site construction, injection operations, and verification of secure storage were evaluated, and mitigation strategies proposed to alleviate those risks.

09 BIOMASS FUELS↗

High-Pressure, High-Temperature Thermal Hydraulic Test Facility for Nuclear-Renewable Hybrid Energy System Studies; Facility Design Description and Status Report

A high-pressure, high-temperature water flow loop has been designed at Idaho National Laboratory (INL) for deployment in the INL Dynamic Energy Transport and Integration Laboratory (DETAIL) within the Energy Systems Laboratory (ESL) D100 northwest high bay. This loop is the first of three thermally coupled flow loops that will comprise the Advanced Reactor Technology Integral System Test (ARTIST) facility. The ARTIST facility will ultimately include a high temperature helium loop and a liquid salt loop, in addition to the PWR loop. The high-pressure water loop will operate at Pressurized Water Reactor (PWR) conditions. It will support experimental research on nuclear-renewable hybrid energy systems as well as advanced reactor technology topics. Within DETAIL, the water flow loop will also serve as a thermal energy source, emulating a reactor system. The loop will be thermally integrated with co-located energy systems including a thermal energy transport loop, thermal energy storage system, and a 25 kW high-temperature electrolysis system for hydrogen production. DETAIL will include additional energy systems such as an integrated microgrid and renewable energy systems including solar photovoltaics. The electrically heated flow loop will be dynamically controlled to simulate nuclear fuel behavior under normal and off-normal operating conditions. DETAIL will be designed for characterization of complex system dynamics. The various components will be interfaced with Digital Real-Time Simulators for supervisory control and dynamic simulation of complete systems. The design and assembly of the high-pressure water flow loop and supporting systems has been subdivided into two Phases. Phase 1, which will be completed by the end of FY17, includes installation of cable trays and supports, electrical conduit, DI water system, drain lift station and the concrete pad for the chiller located outside of the laboratory. Phase 2 includes the detailed design and final assembly of the flow loop, supporting structures and personnel platforms, the chiller and associated piping. As of September, 2017, the final detailed design of the flow loop is complete. Funding for Phase 2 procurement, assembly, system operability checkout, shakedown testing and initial operation of the flow loop is requested for FY18.

42 ENGINEERING↗

Response to External Peer Review Team Report for Corrective Action Unit 97: Yucca Flat/Climax Mine, Nevada National Security Site, Nye County, Nevada, Revision 1

The Underground Test Area (UGTA) Corrective Action Unit (CAU) 97, Yucca Flat/Climax Mine (YF/CM), in the northeast part of the Nevada National Security Site (NNSS) requires environmental corrective action activities to assess contamination resulting from underground nuclear testing. These activities are necessary to comply with the UGTA corrective action strategy defined in Appendix VI, Revision No. 4, of the Federal Facility Agreement and Consent Order (FFACO) (1996, as amended). The Phase I Flow and Transport Model Document for Corrective Action Unit 97: Yucca Flat/Climax Mine, Nevada National Security Site, Nye County, Nevada (N-I, 2013a) was developed and subjected to an external peer review as required by the corrective action investigation (CAI) stage of the UGTA strategy. The YF/CM Peer Review Committee (PRC) raised a number of questions and provided recommendations for supplemental analyses (in the External Peer Review Team Report for Corrective Action Unit 97: Yucca Flat/Climax Mine, Nevada National Security Site, Nye County, Nevada [N-I, 2015]). The purpose of this document is to provide responses to the PRC recommendations addressing the uncertainties identified by the PRC so that sufficient confidence in the contaminant boundary forecasts is established to advance to the Corrective Action Decision Document (CADD)/Corrective Action Plan (CAP) stage and initiate model evaluations. The PRC summarized their concerns and recommendations, and presented discussions of each of these uncertainties in their report (N-I, 2015). The U.S. Department of Energy (DOE), National Nuclear Security Administration Nevada Field Office (NNSA/NFO) responses are summarized in Table ES-1.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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↗

Pretreatments for the continuous production of pyrolytic sugar from lignocellulosic biomass

Fast pyrolysis of lignocellulosic biomass yields little sugar or anhydrosugars compared to pyrolysis of pure polysaccharides because naturally abundant alkali and alkaline earth metals (AAEM) in biomass catalyze the fragmentation of pyranose and furanose rings. Sugar yields can be increased dramatically by pretreating the biomass with sulfuric acid prior to pyrolysis, which passivates the catalytic activity of the metals by converting them into thermally stable salts. However, depolymerization of lignin in biomass also depends on the catalytic activity of AAEM. Thus, passivating AAEM has the unintended consequence of slowing the rate of depolymerization and volatilization of lignin, resulting in a transient melt phase that agglomerates and can foul pyrolysis reactors. Here, to overcome this problem, various non-alkali metal sulfates were tested as replacements for sulfuric acid. Iron in the form of ferrous sulfate proved the most effective in depolymerizing lignin without fragmenting pyranose rings. Conventional nitrogen-blown pyrolysis of ferrous sulfate pretreated corn stover achieved WHSV of 4 h –1 compared to only 0.6 h –1 for acid pretreated corn stover. Autothermal (air-blown) pyrolysis of ferrous sulfate pretreated corn stover showed even more dramatic improvement, increasing WHSV from 1 h –1 to 10 h –1 compared to acid pretreated corn stover under autothermal operation. Fermentable sugar yields from the pyrolysis of corn stover increased from 0.9 wt% to 11.8 wt% on a biomass basis, a 13-fold increase as a result of the ferrous sulfate pretreatment. These advantages combine to increase volumetric sugar productivity from 62 g L –1 h –1 for conventional pyrolysis of untreated corn stover to 2041 g L –1 h –1 for autothermal pyrolysis of ferrous sulfate treated corn stover.

09 BIOMASS FUELS↗

A power compensated differential scanning calorimeter for protein stability characterization

This study presented a power compensated MEMS differential scanning calorimeter (DSC) for protein stability characterization. In this microfabricated sensor, PDMS (Polydimethylsiloxane) and polyimide were used to construct the adiabatic chamber (1 μL) and temperature sensitive vanadium oxide was used as the thermistor material. A power compensation system was implemented to maintain the sample and reference at the same temperature. The resolution study and step response characterization indicated the high sensitivity (6 V/W) and low noise level (60 μk) of the device. The test with IgG1 antibody (mAb1) samples showed clear phase transitions and the data was confirmed to be reasonable by comparing it with the results of commercial DSC’s test. Finally, this device used ~1uL sample amount and could complete the scanning process in 4 min, significantly increasing the throughput of the bimolecular thermodynamics study like drug formulation process.

36 MATERIALS SCIENCE↗