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DOE OSTI2021

Chapter 6 - Polymer and composites additive manufacturing: material extrusion processes

This chapter focuses on material extrusion additive manufacturing (AM) processes for polymers and composite materials. Different extrusion AM platforms, along with their operating mechanism concepts, processing capabilities, and limitations, are discussed here. This chapter also covers state-of-the-art developments in new areas such as hybrid systems, integrated systems, and automation, which facilitate the integration of extrusion-based AM processes into smart manufacturing or Industry 4.0. Following this, a comprehensive discussion on materials development, criteria for successful printing of different materials (thermoplastics, thermosets, and their composites), key factors influencing printing, and material-related challenges in extrusion AM is presented. Finally, a brief overview of current and future potential applications of material extrusion AM technology is provided.

Kishore, Vidya↗

NASA NTRS2007

Process for derivatizing carbon nanotubes with diazonium species

The invention incorporates new processes for the chemical modification of carbon nanotubes. Such processes involve the derivatization of multi- and single-wall carbon nanotubes, including small diameter (ca. 0.7 nm) single-wall carbon nanotubes, with diazonium species. The method allows the chemical attachment of a variety of organic compounds to the side and ends of carbon nanotubes. These chemically modified nanotubes have applications in polymer composite materials, molecular electronic applications and sensor devices. The methods of derivatization include electrochemical induced reactions thermally induced reactions (via in-situ generation of diazonium compounds or pre-formed diazonium compounds), and photochemically induced reactions. The derivatization causes significant changes in the spectroscopic properties of the nanotubes. The estimated degree of functionality is ca. 1 out of every 20 to 30 carbons in a nanotube bearing a functionality moiety. Such electrochemical reduction processes can be adapted to apply site-selective chemical functionalization of nanotubes. Moreover, when modified with suitable chemical groups, the derivatized nanotubes are chemically compatible with a polymer matrix, allowing transfer of the properties of the nanotubes (such as, mechanical strength or electrical conductivity) to the properties of the composite material as a whole. Furthermore, when modified with suitable chemical groups, the groups can be polymerized to form a polymer that includes carbon nanotubes ##STR00001##.

Tour, James M.↗

NASA NTRS2009

Improvements in Production of Single-Walled Carbon Nanotubes

A continuing program of research and development has been directed toward improvement of a prior batch process in which single-walled carbon nanotubes are formed by catalytic disproportionation of carbon monoxide in a fluidized-bed reactor. The overall effect of the improvements has been to make progress toward converting the process from a batch mode to a continuous mode and to scaling of production to larger quantities. Efforts have also been made to optimize associated purification and dispersion post processes to make them effective at large scales and to investigate means of incorporating the purified products into composite materials. The ultimate purpose of the program is to enable the production of high-quality single-walled carbon nanotubes in quantities large enough and at costs low enough to foster the further development of practical applications. The fluidized bed used in this process contains mixed-metal catalyst particles. The choice of the catalyst and the operating conditions is such that the yield of single-walled carbon nanotubes, relative to all forms of carbon (including carbon fibers, multi-walled carbon nanotubes, and graphite) produced in the disproportionation reaction is more than 90 weight percent. After the reaction, the nanotubes are dispersed in various solvents in preparation for end use, which typically involves blending into a plastic, ceramic, or other matrix to form a composite material. Notwithstanding the batch nature of the unmodified prior fluidized-bed process, the fluidized-bed reactor operates in a continuous mode during the process. The operation is almost entirely automated, utilizing mass flow controllers, a control computer running software specific to the process, and other equipment. Moreover, an important inherent advantage of fluidized- bed reactors in general is that solid particles can be added to and removed from fluidized beds during operation. For these reasons, the process and equipment were amenable to modification for conversion from batch to continuous production.

Balzano, Leandro↗

NASA NTRS2003

Composite Development and Applications for RLV Tankage

The development of polymer composite cryogenic tanks is a critical step in creating the next generation of launch vehicles. Future launch vehicles need to minimize the gross liftoff weight (GLOW), which is possible due to the 28%-41% reduction in weight that composite materials can provide over current aluminum technology. The development of composite cryogenic tanks, feedlines, and unpressurized structures are key enabling technologies for performance and cost enhancements for Reusable Launch Vehicles (RLVs). The technology development of composite tanks has provided direct and applicable data for feedlines, unpressurized structures, material compatibility, and cryogenic fluid containment for highly loaded complex structures and interfaces. All three types of structure have similar material systems, processing parameters, scaling issues, analysis methodologies, NDE development, damage tolerance, and repair scenarios. Composite cryogenic tankage is the most complex of the 3 areas and provides the largest breakthrough in technology. A building block approach has been employed to bring this family of difficult technologies to maturity. This approach has built up composite materials, processes, design, analysis and test methods technology through a series of composite test programs beginning with the NASP program to meet aggressive performance goals for reusable launch vehicles. In this paper, the development and application of advanced composites for RLV use is described.

Wright, Richard J.↗

NASA NTRS2003

Flywheels Upgraded for Systems Research

With the advent of high-strength composite materials and microelectronics, flywheels are becoming attractive as a means of storing electrical energy. In addition to the high energy density that flywheels provide, other advantages over conventional electrochemical batteries include long life, high reliability, high efficiency, greater operational flexibility, and higher depths of discharge. High pulse energy is another capability that flywheels can provide. These attributes are favorable for satellites as well as terrestrial energy storage applications. In addition to energy storage for satellites, the several flywheels operating concurrently can provide attitude control, thus combine two functions into one system. This translates into significant weight savings. The NASA Glenn Research Center is involved in the development of this technology for space and terrestrial applications. Glenn is well suited for this research because of its world-class expertise in power electronics design, rotor dynamics, composite material research, magnetic bearings, and motor design and control. Several Glenn organizations are working together on this program. The Structural Mechanics and Dynamics Branch is providing magnetic bearing, controls, and mechanical engineering skills. It is working with the Electrical Systems Development Branch, which has expertise in motors and generators, controls, and avionics systems. Facility support is being provided by the Space Electronic Test Engineering Branch, and the program is being managed by the Space Flight Project Branch. NASA is funding an Aerospace Flywheel Technology Development Program to design, fabricate, and test the Attitude Control/Energy Storage Experiment (ACESE). Two flywheels will be integrated onto a single power bus and run simultaneously to demonstrate a combined energy storage and 1-degree-of-freedom momentum control system. An algorithm that independently regulates direct-current bus voltage and net torque output will be experimentally demonstrated.

Jansen, Ralph H.↗

NASA NTRS2000

Temperature Dependent Modal Test/Analysis Correlation of X-34 Fastrac Composite Rocket Nozzle

A unique high temperature modal test and model correlation/update program has been performed on the composite nozzle of the FASTRAC engine for the NASA X34 Reusable Launch Vehicle. The program was required to provide an accurate high temperature model of nozzle for incorporation into the engine system structural dynamics model for loads calculation; this model is significantly different from the ambient case due to the large decrease in composite material properties due to heating. The modal test was enabled by piggybacking onto a hot-fire test of the nozzle at NASA/Marshall and tracking the natural frequencies as they decreased. A series of high fidelity modal tests and finite element model correlation of the nozzle in a free-free configuration was initially performed. This model was then attached to a modal-test verified model of the engine hot-fire test stand and the' ambient system mode shapes identified. A reduced set of accelerometers was then attached to the nozzle, the engine fired full-duration, and the frequency peaks corresponding to the ambient nozzle modes individually isolated and tracked. To update the finite element model of the nozzle to these frequency curves, a multiplicative factor was. applied to the rate of decline of the composite material property versus temperature table. This new property table was used to create high-temperature nozzle models corresponding to 10 second engine operation increments and tied into the engine system model for loads determination.

Brown, Andrew M.↗

DOE OSTI2026

Promotion of CaCO 3 Nucleation by Carboxyl- and Amine-Terminated Peptoid Nanotubes

The use of surfaces to promote heterogeneous nucleation of CaCO 3 has been extensively studied to better understand natural processes of biomineralization, to develop bioinspired approaches for synthesizing composite materials with diverse functionalities, and as a route toward accelerating CO 2 mineralization. Peptoids have emerged as a material of particular interest, because they offer tunable side chain chemistry while maintaining a constant long-range self-assembled architecture. Here, in this work, we investigate the ability of films of self-assembled -NH 2 and −COOH terminated peptoid nanotubes to promote the nucleation of CaCO 3 . Using a combination of atomic force, scanning electron, and optical microscopy, we find that interwoven films of nanotubes formed from peptoids with -NH 2 side chains promote the preferential formation of vaterite with the (001) plane parallel to the film and exhibit a lower interfacial energy than that reported for inorganic surfaces. In contrast, the film of −COOH-functionalized peptoid nanotubes is a much stronger promoter, giving a particle density 5 orders of magnitude larger than for the -NH 2 terminated peptoid nanotubes and enabling complete coverage of individual peptoid tubes with CaCO 3 nanoparticles that results in a composite material with a 50-fold increase in Young’s modulus. Thus, interwoven films of peptoid nanotubes provide a useful platform for investigating the impact of specific chemical groups on nucleation and offer potential application to accelerated mineralization of CO 2 for removal from the environment or modulation of mineralogy and properties of carbonate-based building materials.

carbon nanotubes↗

NASA NTRS1985

Abrasion behavior of aluminum and composite skin coupons, stiffened skins and stiffened panels representative of transport airplane structures

A three-phase investigation was conducted to compare the friction and wear response of aluminum and graphite-epoxy composite materials when subjected to loading conditions similar to those experienced by the skin panels on the underside of a transport airplane during an emergency belly landing on a runway surface. The first phase involved a laboratory test which used a standard belt sander to provide the sliding abrasive surface. Small skin-coupon test specimens were abraded over a range of pressures and velocities to determine the effects of these variables on the coefficient of friction and wear rate. The second phase involved abrading I-beam stiffened skins on actual runway surface over the same range of pressures and velocities used in the first phase. In the third phase, large stiffened panels which most closely resembled transport fuelage skin construction were abraded on a runway surface. This report presents results from each phase of the investigation and shows comparisons between the friction and wear behavior of the aluminum and graphite-epoxy composite materials.

Jackson, K. E.↗

DOE OSTI2022

Transparent, High‐Charge Capacity Metal Mesh Electrode for Reversible Metal Electrodeposition Dynamic Windows with Dark‐State Transmission <0.1%

Abstract Dynamic windows allow user control over light and heat flow to save energy and maximize comfort. Reversible metal electrodeposition (RME) dynamic windows can uniquely tint to a color‐neutral privacy state (0.1% visible light transmission). The design parameters of transparent metal mesh counter electrodes for high‐contrast RME dynamic windows: high transparency, charge capacity and surface area with low haze, sheet resistance and cost are discussed, concluding that woven metal meshes meet these design parameters. Electroplated current is measured on an indium tin oxide electrode and two meshes with different wire spacings, showing the meshes’ cylindrical geometry enable them to draw more current per square area. The mesh material composition is analyzed to ensure cycling durability in a CuBi electrolyte by developing a transparent mesh with an inert core (stainless steel, SS), a thin Au coating, and a high charge‐capacity (1.5 C cm −2 ) CuBi outer coating. The study demonstrates that the films maintain a consistent Cu:Bi ratio and optical properties after 250 privacy cycles or 1500 cycles to 10% transmission, showing that the Cu and Bi coating is effective in keeping the films from becoming Cu rich with cycling. Finally, a 100 cm 2 device with excellent uniformity and color neutrality is demonstrated.

Yeang, Andrew L.↗

NASA NTRS1993

An overview of the NASA textile composites program

The NASA Langley Research Center is conducting and sponsoring research to explore the benefits of textile reinforced composites for civil transport aircraft primary structures. The objective of this program is to develop and demonstrate the potential of affordable textile reinforced composite materials to meet design properties and damage tolerance requirements of advanced aircraft structures. In addition to in-house research, the program includes major participation by the aircraft industry and aerospace textile companies. The major program elements include development of textile preforms, processing science, mechanics of materials, experimental characterization of materials, and development and evaluation of textile reinforced composite structural elements and subcomponents. The NASA Langley in-house research is focused on science-based understanding of resin transfer molding (RTM), development of powder-coated towpreg processes, analysis methodology, and development of a performance database on textile reinforced composites. The focus of the textile industry participation is on development of multidirectional, damage-tolerant preforms, and the aircraft industry participation is in the areas of innovative design concepts, cost-effective fabrication, and testing of textile reinforced composite structural elements and subcomponents. Textile processes such as 3-D weaving, 2-D and 3-D braiding, and knitting/stitching are being compared with conventional laminated tape processes for improved damage tolerance. Through-the-thickness reinforcements offer significant damage tolerance improvements. However, these gains must be weighed against potential loss in in-plane properties such as strength and stiffness. Analytical trade studies are underway to establish design guidelines for the application of textile material forms to meet specific loading requirements. Fabrication and testing of large structural components are required to establish the full potential of textile reinforced composite materials. The goals of the NASA Langley-sponsored research program are to demonstrate technology readiness with subscale composite components by 1995 and to verify the performance of full-scale composite primary aircraft structural components by 1997. The status of textile reinforced composite structural elements under development by Boeing, Douglas, Lockheed, and Grumman are presented. Included are braided frames and woven/stitched wing and fuselage panels.

Dexter, H. Benson↗

NASA NTRS1995

Load transfer in the stiffener-to-skin joints of a pressurized fuselage

Structural analyses are developed to determine the linear elastic and the geometrically nonlinear elastic response of an internally pressurized, orthogonally stiffened, composite material cylindrical shell. The configuration is a long circular cylindrical shell stiffened on the inside by a regular arrangement of identical stringers and identical rings. Periodicity permits the analysis of a unit cell model consisting of a portion of the shell wall centered over one stringer-ring joint. The stringer-ring-shell joint is modeled in an idealized manner; the stiffeners are mathematically permitted to pass through one another without contact, but do interact indirectly through their mutual contact with the shell at the joint. Discrete beams models of the stiffeners include a stringer with a symmetrical cross section and a ring with either a symmetrical or an asymmetrical open section. Mathematical formulations presented for the linear response include the effect of transverse shear deformations and the effect of warping of the ring's cross section due to torsion. These effects are important when the ring has an asymmetrical cross section because the loss of symmetry in the problem results in torsion and out-of-plane bending of the ring, and a concomitant rotation of the joint at the stiffener intersection about the circumferential axis. Data from a composite material crown panel typical of a large transport fuselage structure are used for two numerical examples. Although the inclusion of geometric nonlinearity reduces the 'pillowing' of the shell, it is found that bending is localized to a narrow region near the stiffener. Including warping deformation of the ring into the analysis changes the sense of the joint rotation. Transverse shear deformation models result in increased joint flexibility.

Johnson, Eric R.↗

DOE OSTI2024

Increased accuracy and signal-to-noise ratio through recent improvements in infra-red video bolometer fabrication and calibration

The infra-red video bolometer (IRVB) is a diagnostic equipped with an infra-red camera that measures the total radiated power in thousands of lines of sight within a large field of view. Recently validated in MAST-U [Fderici et al., Rev. Sci. Instrum. 94, 033502 (2023)], it offers a high spatial resolution map of the radiated power in the divertor region, where large gradients are expected. The IRVB’s sensing element comprises a thin layer of high Z absorbing material, typically platinum, usually coated with carbon to reduce reflections [Peterson et al., Rev. Sci. Instrum. 79, 10E301 (2008)].Here, the possibility of using a relatively inert material such as titanium, is explored that can be produced in layers up to 1 μm compared to 2.5 μm for Pt and then coat it with Pt of the desired thickness (0.3 μm per side here) and carbon. This leads to a higher temperature signal (about 3 times) and better spatial resolution (about 4 times), resulting in higher accuracy in the measured power [Peterson et al., Rev. Sci. Instrum. 79, 10E301 (2008)]. This assembly is also expected to improve foil uniformity, as the Pt layer is obtained via deposition rather than mechanical processes [Mukai et al., Rev. Sci. Instrum. 87, 2014 (2016)].Given its multi-material composition, measuring the thermal properties of the foil assembly is vital. Various methods using a calibrated laser as a heat source have been developed, analyzing the temperature profile shape [Sano et al., Plasma and Fusion Res. 7, 2405039 (2012)] and [Mukai et al., Rev. Sci. Instrum. 89, 10E114 (2018)] or fitting the calculated laser power for different intensities and frequencies [Fderici et al., Rev. Sci. Instrum. 94, 033502 (2023)]. Here, a simpler approach is presented, which relies on analyzing the separate components of the foil heat equation for a single laser exposure in a given area. This can then be iterated over the entire foil to capture local deviations.

Magnetic Fusion Energy↗

NASA NTRS1980

Development of a fire test facility for graphite fiber-reinforced composites

A number of modifications were added to the Model 25 facility to make it specifically applicable for composite material screening tests. Most significant was the development of hardware for trapping fibers released during test and isolating them for quantitative measurement. Capability was added for increasing test section velocities and increasing the range of air/fuel ratios available from very rich to very lean. A provision was added for agitation of the test specimen and the combustion gases by a pulsating gas supply. A variety of specimen configurations was evaluated by an extensive series of tests on a graphite-epoxy reference composite which is representative of material currently used in advanced aircraft. A standard test technique and specimen configuration were established which was satisfactory for the reference composite. A test program was then performed on several alternate composite materials to verify the validity of the test method for relative evaluation of a variety of composite materials.

Alexander, J. G.↗

NASA NTRS1993

Evaluation of advanced materials through experimental mechanics and modelling

Composite materials have been frequently used in aerospace vehicles. Very often defects are inherited during the manufacture and damages are inherited during the construction and services. It becomes critical to understand the mechanical behavior of such composite structure before it can be further used. One good example of these composite structures is the cylindrical bottle of solid rocket motor case with accidental impact damages. Since the replacement of this cylindrical bottle is expensive, it is valuable to know how the damages affects the material, and how it can be repaired. To reach this goal, the damage must be characterized and the stress/strain field must be carefully analyzed. First the damage area, due to impact, is surveyed and identified with a shearography technique which uses the principle of speckle shearing interferometry to measure displacement gradient. Within the damage area of a composite laminate, such as the bottle of solid rocket motor case, all layers are considered to be degraded. Once a lamina being degraded the stiffness as well as strength will be drastically decreased. It becomes a critical area of failure to the whole bottle. And hence the stress/strain field within and around a damage should be accurately evaluated for failure prediction. To investigate the stress/strain field around damages a Hybrid-Numerical method which combines experimental measurement and finite element analysis is used. It is known the stress or strain at the singular point can not be accurately measured by an experimental technique. Nevertheless, if the location is far away from the singular spot, the displacement can be found accurately. Since it reflects the true displacement field locally regardless of the boundary conditions, it is an excellent input data for a finite element analysis to replace the usually assumed boundary conditions. Therefore, the Hybrid-Numerical method is chosen to avoid the difficulty and to take advantage of both experimental technique and finite element analysis. Experimentally, the digital image correlation technique is employed to measure the displacement field. It is done by comparing two digitized images, before and after loading. Numerically, the finite element program, ABAQUS (version 5.2), is used to analyze the stress and strain field. It takes advantage of the high speed and huge memory size of modern supercomputer, CRAY Y-MP, at NASA Marshall Space Flight Center.

Yang, Yii-Ching↗

NASA NTRS1996

Comments on SEE: Comparative Advantages and and Experimental Consequences

The Satellite Energy Exchange experiment measures the periodic, near-miss encounters between a sheppard satellite and a small test body (satellite) in approximately the same orbit about a primary. Several important experimental requirements have been chosen to enhance capabilities: (a) The satellite be flown in a sun-synchronous orbit at an altitude of about 1350 Km, (b) Passive temperature system stabilized by spacecraft axial rotation with sunshade baffles at the end of the spacecraft, (c) Test bodies with different material composition be available for experiments, (d) The containment spacecraft fly about the sheppard mass in a zero-g environment whereas the test bodies, experience average zero-g environment over an orbital period, (e) Primary attitude and station-keeping uses magnetic field alignment plus micro-Newton thrusters such as Field Emission Electric Propulsion, and (f) Very low power (nW) laser tracking systems minimize impulse delivered to test bodies. With the above conditions, SEE has the capabilities: (1) Long duration (several years life-time) flight experiment (2) Long-term, active (with historical time record), self-calibration of satellite mass distribution (capsule geodesy) over lifetime of the spacecraft. (3) Novel passive thermal stabilization systems designed to attain cryogenic temperatures around 78K. (4) Novel spacecraft stabilization systems. (5) Ability to measure G to 1 part in 10(exp 6-7) depending on ultimate duration of experiment. (6) Ability to place limits on both temporal and spacial variations on G. (7) Ability to set experimental limits on the Post Newtonian parameters (PPN) alpha(2) and zeta(2). (8) Ability to measure (or place limits on) the non Einsteinian eccentricity of the Earth-Sun system (and the parameter alpha(1)) for long duration flight. (9) Ability to measure Delta((dot)-G)/G to 1 part in 10(exp 12-13). The MiniSTEP, competes in a limited way with Project SEE. It is designed to improve the measurement of the equivalence principle by seven orders of magnitude using active, low temperature (1.8 K) cooling for SQUID based, differential superconducting circuits. The experiment consists of a small cylinder concentrically located within a larger cylinder at its null gravitational point. The satellite is operated in zero-g mode using four differential accelerometers consisting to two test bodies of different material composition. The SQUIDS are needed to measure test body motion to precisions of 10(exp -18) over a four orbit period. The entire satellite moves in a very precise zero-g mode since the accelerometers are rigidly attached to the satellite. This limits the experiment to an approximately six month due to limitations on helium storage used in cryogenic cooling and thrust control to maintain the zero-g operation.

Smalley, Larry L.↗

NASA NTRS2010

Physical Invariants of Intelligence

A program of research is dedicated to development of a mathematical formalism that could provide, among other things, means by which living systems could be distinguished from non-living ones. A major issue that arises in this research is the following question: What invariants of mathematical models of the physics of systems are (1) characteristic of the behaviors of intelligent living systems and (2) do not depend on specific features of material compositions heretofore considered to be characteristic of life? This research at earlier stages has been reported, albeit from different perspectives, in numerous previous NASA Tech Briefs articles. To recapitulate: One of the main underlying ideas is to extend the application of physical first principles to the behaviors of living systems. Mathematical models of motor dynamics are used to simulate the observable physical behaviors of systems or objects of interest, and models of mental dynamics are used to represent the evolution of the corresponding knowledge bases. For a given system, the knowledge base is modeled in the form of probability distributions and the mental dynamics is represented by models of the evolution of the probability densities or, equivalently, models of flows of information. At the time of reporting the information for this article, the focus of this research was upon the following aspects of the formalism: Intelligence is considered to be a means by which a living system preserves itself and improves its ability to survive and is further considered to manifest itself in feedback from the mental dynamics to the motor dynamics. Because of the feedback from the mental dynamics, the motor dynamics attains quantum-like properties: The trajectory of the physical aspect of the system in the space of dynamical variables splits into a family of different trajectories, and each of those trajectories can be chosen with a probability prescribed by the mental dynamics. From a slightly different perspective, the mechanism of decision-making is feedback from the mental dynamics to the motor dynamics, and this mechanism provides a quantum-like collapse of a random motion into an appropriate deterministic state, such that entropy undergoes a pronounced decrease. The existence of this mechanism is considered to be an invariant of intelligent behavior of living systems, regardless of the origins and material compositions of the systems.

Zak, Michail↗

NASA NTRS2017

High Performance High Temperature Thermoelectric Composites with Metallic Inclusions

The present invention provides a composite thermoelectric material. The composite thermoelectric material can include a semiconductor material comprising a rare earth metal. The atomic percent of the rare earth metal in the semiconductor material can be at least about 20%. The composite thermoelectric material can further include a metal forming metallic inclusions distributed throughout the semiconductor material. The present invention also provides a method of forming this composite thermoelectric material.

Ma, James M.↗

NASA NTRS1992

Recent progress in NASA Langley Research Center textile reinforced composites program

Research was conducted to explore the benefits of textile reinforced composites for transport aircraft primary structures. The objective is to develop and demonstrate the potential of affordable textile reinforced composite materials to meet design properties and damage tolerance requirements of advanced aircraft structural concepts. Some program elements include development of textile preforms, processing science, mechanics of materials, experimental characterization of materials, and development and evaluation of textile reinforced composite structural elements and subcomponents. Textile 3-D weaving, 3-D braiding, and knitting and/or stitching are being compared with conventional laminated tape processes for improved damage tolerance. Through-the-thickness reinforcements offer significant damage tolerance improvements. However, these gains must be weighted against potential loss in in-plane properties such as strength and stiffness. Analytical trade studies are underway to establish design guidelines for the application of textile material forms to meet specific loading requirements. Fabrication and testing of large structural parts are required to establish the potential of textile reinforced composite materials.

Dexter, H. Benson↗