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All sourcesNASA NTRSDOE OSTI
NASA NTRS2022

Run Time Assurance for Electric Vertical Takeoff and Landing Aircraft

NASA is conducting research to demonstrate and evaluate the application of Run Time Assurance (RTA) as a means to assure safety in Electric Vertical Takeoff and Landing (eVTOL) aircraft with highly automated or autonomous flight capability supervised by a single onboard pilot. The work described in this report demonstrates an application of RTA and examines the implications for design and analysis of aircraft functions and systems; aircraft safety hazards; safety assurance; development assurance; and pilot tasks and performance. This research effort also seeks to assess the efficacy of the combined application of traditional Functional Hazard Analysis (FHA) and the more modern System Theoretic Process Analysis (STPA) techniques to perform hazard analyses on aircraft with complex automated and autonomous systems and an onboard pilot. During the research effort we developed architectural designs of two alternate eVTOL aircraft, generally following the process characterized in the SAE standards ARP4754 and ARP4761. The design has focused on the control architectures of these aircraft, which are identical except that one incorporates RTA techniques to reduce the criticality of some key software components. Artifacts of this process include a taxonomy of aircraft-level functions, aircraft-level architecture diagrams, aircraft-level functional hazard assessments (AFHA), function allocations onto aircraft systems and subsystems, functional block diagrams for a select set of control-related functions, and system-level functional hazard assessments (SFHA) for those functions. This project has highlighted the notion that DAL D is something of a sweet spot for low-confidence controllers in an RTA-based design. Among the many activities described in DO-178C, the activities related to requirement verifiability, algorithmic accuracy, and test coverage can be the most challenging for the kinds of advanced control techniques that may be desirable in novel UAM designs, such as adaptive control, machine-learning, artificial intelligence, numerical search, and Monte Carlo based algorithms. Moreover, the standard requires that development teams demonstrate that errors leading to unacceptable failure conditions have been removed from the software. The RTA architecture, which cordons off the low-confidence function, makes it much easier to show this for these kinds of algorithms. With regard to the use of STPA and FHA as complementary hazard analysis techniques, our research effort led us to the conclusion that STPA should be used to derive requirements for hardware and software systems and/or components. Also, STPA is a natural complement to other processes in ARP4754A involving design studies and iteration.

Run-time assurance↗
DOE OSTI2015

SU-C-304-05: Use of Local Noise Power Spectrum and Wavelets in Comprehensive EPID Quality Assurance

Purpose: As EPIDs are increasingly used for IMRT QA and real-time treatment verification, comprehensive quality assurance (QA) of EPIDs becomes critical. Current QA with phantoms such as the Las Vegas and PIPSpro™ can fail in the early detection of EPID artifacts. Beyond image quality assessment, we propose a quantitative methodology using local noise power spectrum (NPS) to characterize image noise and wavelet transform to identify bad pixels and inter-subpanel flat-fielding artifacts. Methods: A total of 93 image sets including bar-pattern images and open exposure images were collected from four iViewGT a-Si EPID systems over three years. Quantitative metrics such as modulation transform function (MTF), NPS and detective quantum efficiency (DQE) were computed for each image set. Local 2D NPS was calculated for each subpanel. A 1D NPS was obtained by radial averaging the 2D NPS and fitted to a power-law function. R-square and slope of the linear regression analysis were used for panel performance assessment. Haar wavelet transformation was employed to identify pixel defects and non-uniform gain correction across subpanels. Results: Overall image quality was assessed with DQE based on empirically derived area under curve (AUC) thresholds. Using linear regression analysis of 1D NPS, panels with acceptable flat fielding were indicated by r-square between 0.8 and 1, and slopes of −0.4 to −0.7. However, for panels requiring flat fielding recalibration, r-square values less than 0.8 and slopes from +0.2 to −0.4 were observed. The wavelet transform successfully identified pixel defects and inter-subpanel flat fielding artifacts. Standard QA with the Las Vegas and PIPSpro phantoms failed to detect these artifacts. Conclusion: The proposed QA methodology is promising for the early detection of imaging and dosimetric artifacts of EPIDs. Local NPS can accurately characterize the noise level within each subpanel, while the wavelet transforms can detect bad pixels and inter-subpanel flat fielding artifacts.

60 APPLIED LIFE SCIENCES↗
NASA NTRS2017

R2U2: Tool Overview

R2U2 (Realizable, Responsive, Unobtrusive Unit) is an extensible framework for runtime System HealthManagement (SHM) of cyber-physical systems. R2U2 can be run in hardware (e.g., FPGAs), or software; can monitorhardware, software, or a combination of the two; and can analyze a range of different types of system requirementsduring runtime. An R2U2 requirement is specified utilizing a hierarchical combination of building blocks: temporal formula runtime observers (in LTL or MTL), Bayesian networks, sensor filters, and Boolean testers. Importantly, the framework is extensible; it is designed to enable definitions of new building blocks in combination with the core structure. Originally deployed on Unmanned Aerial Systems (UAS), R2U2 is designed to run on a wide range of embedded platforms, from autonomous systems like rovers, satellites, and robots, to human-assistive ground systems and cockpits. R2U2 is named after the requirements it satisfies; while the exact requirements vary by platform and mission, the ability to formally reason about realizability, responsiveness, and unobtrusiveness is necessary for flight certifiability, safety-critical system assurance, and achievement of technology readiness levels for target systems. Realizability ensures that R2U2 is suficiently expressive to encapsulate meaningful runtime requirements while maintaining adaptability to run on different platforms, transition between different mission stages, and update quickly between missions. Responsiveness entails continuously monitoring the system under test, real-time reasoning, reporting intermediate status, and as-early-as-possible requirements evaluations. Unobtrusiveness ensures compliance with the crucial properties of the target architecture: functionality, certifiability, timing, tolerances, cost, or other constraints.

Rozier, Kristin Y.↗
DOE OSTI2014

Poster — Thur Eve — 40: Automated Quality Assurance for Remote-Afterloading High Dose Rate Brachytherapy

High dose rate (HDR) remote afterloading brachytherapy involves sending a small, high-activity radioactive source attached to a cable to different positions within a hollow applicator implanted in the patient. It is critical that the source position within the applicator and the dwell time of the source are accurate. Daily quality assurance (QA) tests of the positional and dwell time accuracy are essential to ensure that the accuracy of the remote afterloader is not compromised prior to patient treatment. Our centre has developed an automated, video-based QA system for HDR brachytherapy that is dramatically superior to existing diode or film QA solutions in terms of cost, objectivity, positional accuracy, with additional functionalities such as being able to determine source dwell time and transit time of the source. In our system, a video is taken of the brachytherapy source as it is sent out through a position check ruler, with the source visible through a clear window. Using a proprietary image analysis algorithm, the source position is determined with respect to time as it moves to different positions along the check ruler. The total material cost of the video-based system was under $20, consisting of a commercial webcam and adjustable stand. The accuracy of the position measurement is ±0.2 mm, and the time resolution is 30 msec. Additionally, our system is capable of robustly verifying the source transit time and velocity (a test required by the AAPM and CPQR recommendations), which is currently difficult to perform accurately.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2014

Statistical Hot Channel Analysis for the NBSR

A statistical analysis of thermal limits has been carried out for the research reactor (NBSR) at the National Institute of Standards and Technology (NIST). The objective of this analysis was to update the uncertainties of the hot channel factors with respect to previous analysis for both high-enriched uranium (HEU) and low-enriched uranium (LEU) fuels. Although uncertainties in key parameters which enter into the analysis are not yet known for the LEU core, the current analysis uses reasonable approximations instead of conservative estimates based on HEU values. Cumulative distribution functions (CDFs) were obtained for critical heat flux ratio (CHFR), and onset of flow instability ratio (OFIR). As was done previously, the Sudo-Kaminaga correlation was used for CHF and the Saha-Zuber correlation was used for OFI. Results were obtained for probability levels of 90%, 95%, and 99.9%. As an example of the analysis, the results for both the existing reactor with HEU fuel and the LEU core show that CHFR would have to be above 1.39 to assure with 95% probability that there is no CHF. For the OFIR, the results show that the ratio should be above 1.40 to assure with a 95% probability that OFI is not reached.

42 ENGINEERING↗
NASA NTRS2015

Risky Business

During my internship I worked on two major projects, recommending improvements for the Center's Risk Management Workshop and helping with the strategic planning efforts for Safety and Mission Assurance (S&MA). The risk management improvements is the key project I worked on this semester through my internship, while the strategic planning is the secondary assignment. S&MA Business Office covers both aspects in its delegation, getting both spans some of the work done in the office. A risk is a future event with a negative consequence that has some probability of occurring. Safety and Mission Assurance identifies, analyzes, plans, and tracks risk. The directorate offers the Center a Risk Management Workshop, and part of the ongoing efforts of S&MA is to make continuous improvements to the RM Workshop. By using the Project Management Institute's (PMI) Standard for Risk Management, I performed a gap analysis to make improvements for our materials. I benchmarked the PMI's Risk Management Standard, compared our Risk Management Workshop materials to PMI's standard, and identified any gaps in our material. My major findings were presented to the Business Office of S&MA for a decision on whether or not to incorporate the improvements. These suggestions were made by attending JSC working group meetings, Health, Safety and Environment (HSE) panel reviews and various risk review meetings. The improvements provide better understanding of risk management processes and enhanced risk tracking knowledge and skills. Risk management is an integral part of any engineering discipline, getting exposed to this section of engineering will greatly help shape my career in the future. Johnson Space Center is a world leader in risk management processes; learning risk management here gives me a huge advantage over my peers, as well as understanding decision making in the context of risk management will help me to be a well-rounded engineer. Strategic planning is an area I had not previously studied. Helping with the strategic planning efforts in S&MA has taught me how organizations think and function as a whole. S&MA is adopting a balanced scorecard approach to strategic planning. As part of this planning method strategic themes, objectives, and initiatives are formed. I attended strategic theme team workshops that formed the strategy map for the directorate and gave shape to the plan. Also during these workshops the objectives were discussed and built. Learning the process for strategic planning has helped me better understand how organizations and businesses function, which also helps me to be a more effective employee. Other assignments I had during my internship included completing the Safety and Mission Assurance Technical Excellent Program (STEP) Level 1, as well as doing a two week rotation through the Space Exploration division in S&MA, specifically working with a thermal protection systems (TPS) engineer. While working there, I learned about the Orion capsule and the SpaceX Dragon cargo capsule. I attended meetings to prepare the engineers for the upcoming Critical Design Reviews for both capsules and reviewed test data. Learning risk management, strategic planning, and working in the Space Exploration division has taught me about many aspects of S&MA. My internship at NASA has given me new experiences and taught me numerous subjects that I would have otherwise not learned. This opportunity has expanded my educational horizons and is helping me to become a more useful engineer and employee.

Yarbrough, Katherine↗
DOE OSTI2024

Development of an Optical Library for Coevaporated CdSe x Te 1– x

The conversion efficiency of CdTe solar cells may be improved by bandgap engineering, i.e., changing the bandgap value through the addition of Se in the absorber. The Se alloying enables a short-circuit current density improvement, as it leads to a bandgap energy value decrease. Furthermore, it has been associated with increased minority carrier lifetimes, assuring high open-circuit voltage values. An Se gradient profile control can further optimize the solar cell performance. Thus, an optical model baseline of the CdSe x Te 1–x (CST) compound was developed. Spectroscopic ellipsometry measurements were conducted to accurately extract the optical constants of ten CST layers deposited through coevaporation with x varying from 0 to 1. Using the measured dielectric function spectra from the discrete CST layers with varying x, and considering the composition-induced shift in the critical point energies, an energy-shift model was employed to develop the accurate optical library for the CST compound for any x value to provide data for future modeling and optimization. Furthermore, the library accuracy was validated through optical simulations of the quantum efficiency of a graded CST solar cell using the finite-difference time-domain method by replicating the Se profile in the absorber layer measured through secondary ion mass spectrometry.

14 SOLAR ENERGY↗
NASA NTRS1992

Microbiology operations and facilities aboard restructured Space Station Freedom

With the restructure and funding changes for Space Station Freedom, the Environmental Health System (EHS)/Microbiology Subsystem revised its scheduling and operational requirements for component hardware. The function of the Microbiology Subsystem is to monitor the environmental quality of air, water, and internal surfaces and, in part, crew health on board Space Station. Its critical role shall be the identification of microbial contaminants in the environment that may cause system degradation, produce unsanitary or pathogenic conditions, or reduce crew and mission effectiveness. EHS/Microbiology operations and equipment shall be introduced in concert with a phased assembly sequence, from Man Tended Capability (MTC) through Permanently Manned Capability (PMC). Effective Microbiology operations and subsystem components will assure a safe, habitable, and useful spacecraft environment for life sciences research and long-term manned exploration.

Cioletti, Louis A.↗
DOE OSTI2020

Highly Available Nuclear Power for Mission-Critical Applications

Some energy consumers require power on an anytime, all-year-round basis with a high level of certainty, including defense installations, isolated communities, and some industrial processes. For these customers, interruptions in electricity or heat can mean substantial financial loss or even loss of life. In the absence of grid-scale energy storage, a high level of power availability can be accomplished only through the robustness and redundancy of power generators. The NuScale small modular reactor design is well suited to provide highly available power because of several features related to both the nuclear steam supply system and the overall plant design. In analogy to Redundant Array of Independent Disks (RAID) systems used to provide highly reliable data storage, a NuScale plant can assure sustained power generation by virtue of its Redundant Array of Integral Reactors (RAIR).This paper describes the NuScale RAIR plant features and summarizes the results of a rigorous analysis of RAIR availability as a function of power or, conversely, the RAIR plant output power as a function of power availability. The analysis utilized the Matrix Laboratory code (MATLAB) and included probability distributions for the frequency and duration of module outages due to planned and unplanned events. Further, the study evaluated the impact of implementing turbine bypass rather than module shutdown and using one or more modules to supply house loads in the case of loss of off-site power (LOOP). Availability results are presented for a 12-module RAIR plant with and without turbine bypass enabled during a LOOP and for different possible connections to the off-site power distribution grid and dedicated service loads. Results indicate that a very high level of availability can be achieved at relatively high power output levels, regardless of turbine bypass and dedicated load connection, compared to the operating fleet.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRS2007

A Distributed Trajectory-Oriented Approach to Managing Traffic Complexity

In order to handle the expected increase in air traffic volume, the next generation air transportation system is moving towards a distributed control architecture, in which ground-based service providers such as controllers and traffic managers and air-based users such as pilots share responsibility for aircraft trajectory generation and management. While its architecture becomes more distributed, the goal of the Air Traffic Management (ATM) system remains to achieve objectives such as maintaining safety and efficiency. It is, therefore, critical to design appropriate control elements to ensure that aircraft and groundbased actions result in achieving these objectives without unduly restricting user-preferred trajectories. This paper presents a trajectory-oriented approach containing two such elements. One is a trajectory flexibility preservation function, by which aircraft plan their trajectories to preserve flexibility to accommodate unforeseen events. And the other is a trajectory constraint minimization function by which ground-based agents, in collaboration with air-based agents, impose just-enough restrictions on trajectories to achieve ATM objectives, such as separation assurance and flow management. The underlying hypothesis is that preserving trajectory flexibility of each individual aircraft naturally achieves the aggregate objective of avoiding excessive traffic complexity, and that trajectory flexibility is increased by minimizing constraints without jeopardizing the intended ATM objectives. The paper presents conceptually how the two functions operate in a distributed control architecture that includes self separation. The paper illustrates the concept through hypothetical scenarios involving conflict resolution and flow management. It presents a functional analysis of the interaction and information flow between the functions. It also presents an analytical framework for defining metrics and developing methods to preserve trajectory flexibility and minimize its constraints. In this framework flexibility is defined in terms of robustness and adaptability to disturbances and the impact of constraints is illustrated through analysis of a trajectory solution space with limited degrees of freedom and in simple constraint situations involving meeting multiple times of arrival and resolving a conflict.

Idris, Husni↗
NASA NTRS2016

Flat H Frangible Joint Evolution

Space vehicle staging and separation events require pyrotechnic devices. They are single-use mechanisms that cannot be tested, nor can failure-tolerant performance be demonstrated in actual flight articles prior to flight use. This necessitates the implementation of a robust design and test approach coupled with a fully redundant, failure-tolerant explosive mechanism to ensure that the system functions even in the event of a single failure. Historically, NASA has followed the single failure-tolerant (SFT) design philosophy for all human-rated spacecraft, including the Space Shuttle Program. Following the end of this program, aerospace companies proposed building the next generation human-rated vehicles with off-the-shelf, non-redundant, zero-failure-tolerant (ZFT) separation systems. Currently, spacecraft and launch vehicle providers for both the Orion and Commercial Crew Programs (CCPs) plan to deviate from the heritage safety approach and NASA's SFT human rating requirements. Both programs' partners have base-lined ZFT frangible joints for vehicle staging and fairing separation. These joints are commercially available from pyrotechnic vendors. Non-human-rated missions have flown them numerous times. The joints are relatively easy to integrate structurally within the spacecraft. In addition, the separation event is debris free, and the resultant pyro shock is lower than that of other design solutions. It is, however, a serious deficiency to lack failure tolerance. When used for critical applications on human-rated vehicles, a single failure could potentially lead to loss of crew (LOC) or loss of mission (LOM)). The Engineering and Safety & Mission Assurance directorates within the NASA Johnson Space Center took action to address this safety issue by initiating a project to develop a fully redundant, SFT frangible joint design, known as the Flat H. Critical to the ability to retrofit on launch vehicles being developed, the SFT mechanisms must fit within the same three-dimensional envelope as current designs as well as meet structural loads requirements. There is increased mass associated with the redundant design, and the goal is to minimize the weight impact as much as possible. These requirements presented significant challenges, both technically and financially; these challenges will be explored in this paper. Perhaps greater than the technical issues confronted during this design process, were the financial considerations. These were a significant part of the story of this design and development plan. Insufficient financial and labor resources were formidable barriers to completing this project. Nevertheless, JSC personnel successfully conducted several test series at JSC with very useful results. The many lessons learned drove design improvements, performance efficiency, and increased functional reliability. This paper examines the significant technical and financial challenges that these requirements posed to the project team. It discusses the evolution of the SFT frangible joint design, including optimization, testing, and successful partnering of the Johnson Space Center (JSC) engineering and JSC safety organizations, to enhance the flight safety margin for America's next generation of human-rated space vehicles.

Diegelman, Thomas E.↗
DOE OSTI2020

Structural modeling and dynamic analysis of condensate storage tanks in nuclear power plants

Condensate storage tanks (CSTs) in nuclear power plants (NPPs) are classified as critical equipment capable of surviving strong shaking in a design basis earthquake to assure the ability to subsequently provide cooling water. Structural modeling and dynamic analysis of CSTs are complicated due to fluid-structure interaction (FSI) and coupling issues, which could have significant effects on seismic response. The capability of a number of approximate models to capture seismic response is investigated using dynamic analysis results from detailed finite element models. Modal analyses and time history analyses are carried out using both 2D and 3D models to predict the dynamic behavior of CSTs as a function of ground motion intensity. Although 2D simplified models can be used to quickly evaluate the dynamic response of CSTs when there is substantial margin to failure, a detailed 3D model is required when it is necessary to examine a limit state associated with the failure mode of the tank. The findings show good agreement between the natural frequencies of convective modes determined from the 2D and 3D CST models. The difference between the frequencies of impulsive modes were found to be equal to or less than 25%.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
DOE OSTI2025

The AMACStar ASIC for the HL-LHC ATLAS ITk Strip detector: design, verification, testing, and quality assurance

For the high-luminosity upgrade to the LHC (HL-LHC), the ATLAS detector at CERN requires an all-new inner detector, the Inner Tracker (ITk). The ITk Strip subdetector is made up of silicon modules, which include three types of radiation-hard ASICs. One of these is the Autonomous Monitor and Control (AMAC). The AMAC is manufactured by Global Foundries using 130 nm CMOS8RF DM technology and is approximately 3 by 5 mm in size. This ASIC autonomously monitors the temperatures, voltages, and currents in the module components while controlling critical values in order to prevent these quantities from reaching dangerous levels. The final design, AMACStar, was verified, tested, and ensured to perform all necessary functions. A quality control procedure using an in-house probe station set-up was developed in order to ensure that every individual chip on each wafer of AMACStars required by the ITk Strip project met performance requirements. The average per wafer yield of usable AMACStars is 92.33%, exceeding the design-specific 90% yield estimated for project costing. This estimate was based on actual yields for similar designs in this process.

Analogue electronic circuits↗
NASA NTRS1999

A Methodology for Writing High Quality Requirements Specification and Evaluating Existing Ones

Requirements development and management have always been critical in the implementation of software systems; engineers are unable to build what analysts can't define. It is generally accepted that the earlier in the life cycle potential risks are identified the easier it is to eliminate or manage the conditions that introduce that risk. Problems that are not found until testing are approximately 14 times more costly to fix than if the problem was found in the requirement phase. The requirements specification, as the first tangible representation of the capability to be produced, establishes the basis for all of the project's engineering management and assurance functions. If the quality of the requirements specification is poor it can give rise to risks in all areas of the project. Recently, automated tools have become available to support requirements management. The use of these tools not only provides support in the definition and tracing of requirements, but it also opens the door to effective use of metrics in characterizing and assessing the quality of the requirement specifications.

Rosenberg, Linda↗
NASA NTRS2001

Reducing Bolt Preload Variation with Angle-of-Twist Bolt Loading

Critical high-pressure sealing joints on the Space Shuttle reusable solid rocket motor require precise control of bolt preload to ensure proper joint function. As the reusable solid rocket motor experiences rapid internal pressurization, correct bolt preloads maintain the sealing capability and structural integrity of the hardware. The angle-of-twist process provides the right combination of preload accuracy, reliability, process control, and assembly-friendly design. It improves significantly over previous methods. The sophisticated angle-of-twist process controls have yielded answers to all discrepancies encountered while the simplicity of the root process has assured joint preload reliability.

Thompson, Bryce↗
DOE OSTI2010

Applying Human Factors during the SIS Life Cycle

Safety Instrumented Systems (SIS) are widely used in U.S. Department of Energy's (DOE) nonreactor nuclear facilities for safety-critical applications. Although use of the SIS technology and computer-based digital controls, can improve performance and safety, it potentially introduces additional complexities, such as failure modes that are not readily detectable. Either automated actions or manual (operator) actions may be required to complete the safety instrumented function to place the process in a safe state or mitigate a hazard in response to an alarm or indication. DOE will issue a new standard, Application of Safety Instrumented Systems Used at DOE Nonreactor Nuclear Facilities, to provide guidance for the design, procurement, installation, testing, maintenance, operation, and quality assurance of SIS used in safety significant functions at DOE nonreactor nuclear facilities. The DOE standard focuses on utilizing the process industry consensus standard, American National Standards Institute/ International Society of Automation (ANSI/ISA) 84.00.01, Functional Safety: Safety Instrumented Systems for the Process Industry Sector, to support reliable SIS design throughout the DOE complex. SIS design must take into account human-machine interfaces and their limitations and follow good human factors engineering (HFE) practices. HFE encompasses many diverse areas (e.g., information display, user-system interaction, alarm management, operator response, control room design, and system maintainability), which affect all aspects of system development and modification. This paper presents how the HFE processes and principles apply throughout the SIS life cycle to support the design and use of SIS at DOE nonreactor nuclear facilities.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1999

A Methodology for Writing High Quality Requirement Specifications and for Evaluating Existing Ones

Requirements development and management have always been critical in the implementation of software systems-engineers are unable to build what analysts can not define. It is generally accepted that the earlier in the life cycle potential risks are identified the easier it is to eliminate or manage the conditions that introduce that risk. Problems that are not found until testing are approximately 14 times more costly to fix than if the problem was found in the requirement phase. The requirements specification, as the first tangible representation of the capability to be produced, establishes the basis for all of the project's engineering management and assurance functions. If the quality of the requirements specification is poor it can give rise to risks in all areas of the project. Recently, automated tools have become available to support requirements management. The use of these tools not only provides support in the definition and tracing of requirements, but it also opens the door to effective use of metrics in characterizing and assessing the quality of the requirement specifications.

Rosenberg, Linda↗
DOE OSTI2012

Polymer/organosilica nanocomposites based on polyimide with benzimidazole linkages and reactive organoclay containing isoleucine amino acid: Synthesis, characterization and morphology properties

Highlights: ► A reactive organoclay was formed using L-isoleucine amino acid as a swelling agent. ► Polyimide was synthesized from benzimidazole diamine and pyromellitic dianhydride. ► Imide and benzimidazole groups assured the thermal stability of the nanocomposites. ► Nanocomposite films were prepared by an in situ polymerization reaction. ► The TEM micrographs of nanocomposites revealed well-exfoliated structures. -- Abstract: Polyimide–silica nanocomposites are attractive hybrid architectures that possess excellent mechanical, thermal and chemical properties. But, the dispersion of inorganic domains in the polymer matrix and the compatibility between the organic and inorganic phases are critical factors in these hybrid systems. In this investigation, a reactive organoclay was prepared via ion exchange reaction between protonated form of difunctional L-isoleucine amino acid as a swelling agent and Cloisite Na{sup +} montmorillonite. Amine functional groups of this swelling agent formed an ionic bond with the negatively charged silicates, whereas the remaining acid functional groups were available for further interaction with polymer chains. Then organo-soluble polyimide (PI) have been successfully synthesized from the reaction of 2-(3,5-diaminophenyl)-benzimidazole and pyromellitic dianhydride in N,N-dimethylacetamide. Finally, PI/organoclay nanocomposite films enclosing 1%, 3%, 5%, 7% and 10% of synthesized organoclay were successfully prepared by an in situ polymerization reaction through thermal imidization. The synthesized hybrid materials were subsequently characterized by Fourier transform infrared spectroscopy, X-ray diffraction, electron microscopy, and thermogravimetric analysis techniques. The PI/organoclay nanocomposite films have good optical transparencies and the mechanical properties were substantially improved by the incorporation of the reactive organoclay.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗