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At least 19 records

Controlled Contamination of Epoxy Composites with PDMS and Removal by Laser Ablation

Surface preparation is critical to the performance of adhesively bonded composites. During manufacturing, minute quantities of mold release compounds are inevitably deposited on faying surfaces and may compromise bond performance. To ensure safety, mechanical fasteners and other crack arrest features must be installed in the bondlines of primary structures, which negates some advantages of adhesively bonded construction. Laser ablation is an automated, repeatable, and scalable process with high potential for the surface preparation of metals and composites in critical applications such as primary airframe structures. In this study, laser ablation is evaluated on composite surfaces for the removal of polydimethylsiloxane (PDMS), a common mold release material. Composite panels were contaminated uniformly with PDMS film thicknesses as low as 6.0 nm as measured by variable angle spectroscopic ellipsometry. Bond performance was assessed by mechanical testing using a 250 F cure, epoxy adhesive and compared with pre-bond surface inspection results. Water contact angle, optically stimulated electron emission, and laser induced breakdown spectroscopy were used to characterize contaminated and laser ablated surfaces. The failure mode obtained from double cantilever beam tests correlated well with surface characterization data. The test results indicated that even low levels of PDMS were not completely removed by laser ablation.

Palmieri, Frank↗

Relationship of Cure Temperature to Mechanical, Physical, and Dielectric Performance of PDMS Glass Composite for Electric Motor Insulation

Achieving NASAs aggressive fuel burn and emission reduction for N-plus-3 aircraft will require hybrid electric propulsion system in which electric motors driven by either power generated from turbine or energy storage system will power the fan for propulsion. Motors designed for hybrid electric aircraft are expected to operate at medium to high voltages over long durations in a high altitude service environment. Such conditions have driven research toward the development of wire insulation with improved mechanical strength, thermal stability and increased breakdown voltage. The silicone class of materials has been considered for electric wire insulation due to its inherent thermal stability, dielectric strength and mechanical integrity. This paper evaluates the dependence of these properties on the cure conditions of a polydimethyl-siloxane (PDMS) elastomer; where both cure temperature and base-to-catalyst ratio were varied. The PDMS elastomer was evaluated as a bulk material and an impregnation matrix within a lightweight glass veil support. The E-glass support was selected for mechanical stiffness and dielectric strength. This work has shown a correlation between cure conditions and material physical properties. Tensile strength increased with cure temperature whereas breakdown voltage tended to be independent of process variations. The results will be used to direct material formulation based on specific insulation requirements.

insulation↗

Spectral Polarization Distribution Models (PDMs) for NASA CLARREO Pathfinder’s Inter-Calibration Applications

Solar radiation scattered by Earth surfaces of various scene types such as oceans, deserts, tree leaves etc and atmospheric molecules and particles is polarized and the amount of polarization depends on the surface composition and particle physical properties. This can be a source of measurement errors in satellite data if a non-polarimetric radiometric sensor is sensitive to the polarization state of light. To obtain highly accurate spectral solar radiation data from the Earth-atmosphere system for the space-borne inter-calibration studies as proposed in NASA's Climate Absolute Radiance and Refractivity Observatory (CLARREO) mission and the CLARREO Pathfinder (CPF) mission, the spectral polarization state of the reflected solar light at the top of atmosphere (TOA) must be known with sufficient accuracy. The degree of polarization (DOP) and the angle of linear polarization (AOLP) of the light at the TOA as functions of incident and viewing geometry and scene type construct the Polarization Distribution Models (PDMs) for correction of polarization-induced error of satellite data. In this work, algorithms for modeling the spectral polarization state of reflected sunlight from various types of Earth, including oceans, deserts, vegetated land surfaces and these scene types with all kinds of clouds, are developed. By comparing the model results with the PARASOL satellite data, our numerical results demonstrate that the model can provide a reliable approach for making the spectral PDMs for wavelengths between 320 and 2300 nm for satellite inter-calibration applications as proposed in the CLARREO and the CLARREO CPF missions.

Sun, Wenbo↗

Process Development for Removal of Siloxanes from ISS Atmosphere

Dimethylsilanediol (DMSD) has been identified as a problematic organic contaminant aboard the ISS. This contaminant was initially identified in humidity condensate and in the Water Processor Assembly (WPA) product water in 2010 when routine water quality monitoring an increasing total organic carbon (TOC) trend in the WPA product water. Although DMSD is not a crew health hazard at the levels observed in the product water, it can degrade the WPA catalytic reactor's effectiveness and cause early replacement of Multifiltration Beds. DMSD may also degrade the performance of the Oxygen Generation System (OGS) which uses the WPA product water for electrolysis. An investigation into the source of DMSD has determined that polydimethylsiloxane (PDMS) compounds are likely hydrolyzing in the Condensing Heat Exchangers (CHX) to form DMSD. PDMS compounds are prevalent aboard ISS from a variety of sources, including crew hygiene products, adhesives, caulks, lubricants, and various nonmetallic materials. PDMS compounds are also known to contribute to CHX hydrophilic coating degradation by rendering it hydrophobic and therefore adversely affecting its ability to effectively transmit water to the condensate bus. Eventually this loss in performance results in water droplets in the air flow exiting the CHX, which may lead to microbial growth in the air ducts and may impact the performance of downstream systems. Several options have been evaluated to address these concerns. Modifications to the Water Processor Multifiltration Beds and Catalytic Reactor for removal of DMSD were not considered viable, and did not address the issue with PDMS compound degradation of the CHX coating. Design concepts are now in development for removing PDMS compounds from the air stream before they can reach the CHX coating, thus preventing coating degradation and hydrolysis of the PDMS compounds to DMSD. This paper summarizes the current status of the effort to treat these contaminants on ISS.

Carter, Layne↗

Surface Monitoring of CFRP Structures for Adhesive Bonding

Adhesive bonding of composite materials requires reliable monitoring and detection of surface contaminants to assure robust and durable bonded structures. Surface treatment and effective monitoring prior to bonding is essential in order to obtain a surface free from contaminants that may degrade structural performance. Two techniques which monitor the effectiveness of the laser surface treatment of carbon fiber reinforced polymer (CFRP) materials are being investigated: laser induced breakdown spectroscopy (LIBS) and optically stimulated electron emission (OSEE). The applicability of LIBS to detect silicone contaminants on CFRP composites is studied using ~35 ns Nd:YAG laser pulses at 355 nm with a pulse energy of 45 mJ. The LIBS regime in which pulse energies are < 100 mJ is referred to as mLIBS. CFRP surfaces were contaminated with polydimethylsiloxane (PDMS), a major component of silicone based mold release agents. The presence of PDMS is found by inspecting the Si I emission line at 288.2 nm. Untreated CFRP samples and CFRP contaminated with PDMS were tested. The PDMS areal density ranged from 0.36 Â+/- 0.04 to 0.51 Â+/- 0.16 mg/cm2. The results demonstrate the successful detection of PDMS on CFRP using mLIBS. In addition, OSEE was used to measure CFRP surface cleanliness pre- and post-treatment by laser ablation on specimens contaminated with PDMS coatings from 8 nm to 1311 nm in thickness. The results showed a significant increase in the OSEE photocurrent after laser surface treatment.

Ledesma, Rodolfo↗

Copoly(Imide Siloxane) Abhesive Materials with Varied Siloxane Oligomer Length

Incorporation of PDMS moieties into a polyimide matrix lowered the surface energy resulting in enhanced adhesive interactions. Polyimide siloxane materials were generated using amine-terminated PDMS oligomers of different lengths to study changes in surface migration behavior, phase segregation, mechanical, thermal, and optical properties. These materials were characterized using contact angle goniometry, tensile testing, and differential scanning calorimetry. The surface migration behavior of the PDMS component depended upon the siloxane molecular weight as indicated by distinct relationships between PDMS chain length and advancing water contact angles. Similar correlations were observed for percent elongation values obtained from tensile testing, while the addition of PDMS reduced the modulus. High fidelity topographical modification via laser ablation patterning further reduced the polyimide siloxane surface energy. Initial particulate adhesion testing experiments demonstrated that polyimide siloxane materials exhibited greater abhesive interactions relative to their respective homopolyimides.

Wohl, Christopher J.↗

Microfluidic Pumps Containing Teflon [Trademark] AF Diaphragms

Microfluidic pumps and valves based on pneumatically actuated diaphragms made of Teflon AF polymers are being developed for incorporation into laboratory-on-a-chip devices that must perform well over temperature ranges wider than those of prior diaphragm-based microfluidic pumps and valves. Other potential applications include implanted biomedical microfluidic devices, wherein the biocompatability of Teflon AF polymers would be highly advantageous. These pumps and valves have been demonstrated to function stably after cycling through temperatures from -125 to 120 C. These pumps and valves are intended to be successors to similar prior pumps and valves containing diaphragms made of polydimethylsiloxane (PDMS) [commonly known as silicone rubber]. The PDMS-containing valves ae designed to function stably only within the temperature range from 5 to 80 C. Undesirably, PDMS membranes are somwehat porous and retain water. PDMS is especially unsuitable for use at temperatures below 0 C because the formation of ice crystals increases porosity and introduces microshear.

Willis, Peter↗

Elastomeric Sensing of Pressure with Liquid Metal and Wireless Inductive Coupling

This project describes resistance-based soft sensors filled with liquid metal, which permit measurements of large strains (0 percent to 110 percent), associated with small forces of less than 30 Newtons. This work also demonstrates a methodology for wireless transfer of these strain measurements without connected electrodes. These sensors allow intermittent detection of pressure on soft membranes with low force. Adapting these sensors for passive wireless pressure sensing will eliminate the need for embedded batteries, and will allow the sensors to transmit pressure data through non-conductive materials including glass and acrylic. The absence of batteries allows us to embed these sensors into materials for long-term use because the sensors only use passive analog circuit elements. We found the oxidation of the liquid metal (eutectic gallium indium) plays a role in the repeatability of the soft sensors. We investigated how the oxidation layer affected the behavior of the sensor by encapsulating materials (silicone, fluorosilicone, and PVC) with varied permeabilities to oxygen. We measured the effects of mechanical loading on the oxidation layer and the effects of wireless inductive coupling on the oxidation layer. We concluded our research by investigating the effects of embedding self-resonant circuits into polydimethylsiloxane (PDMS). Efforts to design engineered systems with soft materials are a growing field with progress in soft robotics, epidermal electronics, and wearable electronics. In the field of soft robotics, PDMS-based grippers are capable of picking up delicate objects because their form-fitting properties allow them to conform to the shape of objects more easily than conventional robotic grippers. Epidermal devices also use PDMS as a substrate to hold electronic components such as radios, sensors, and power supply circuits. Additionally, PDMS-based soft sensors can monitor human motion with liquid metal embedded within micro-channels. Passive wireless sensors have applications in structural health monitoring and medical health monitoring. Doctors can take wireless blood pressure measurements inside arteries to monitor the progression of heart disease. Glaucoma patients can use this technology to monitor the pressure in their eyes to track the progression of the disease.

Dick, Jacob↗

Surface Characterization of Carbon Fiber Reinforced Polymers by Picosecond Laser Induced Breakdown Spectroscopy

Adhesive bonding of composite materials requires reliable monitoring and detection of surface contaminants as part of a vigorous quality control process to assure robust and durable bonded structures. Surface treatment and effective monitoring prior to bonding are essential in order to obtain a surface which is free from contaminants that may lead to inferior bond quality. In this study, the focus is to advance the laser induced breakdown spectroscopy (LIBS) technique by using pulse energies below 100 μJ (μLIBS) for the detection of low levels of silicone contaminants in carbon fiber reinforced polymer (CFRP) composites. Various CFRP surface conditions were investigated by LIBS using ∼10 ps, 355 nm laser pulses with pulse energies below 30 μJ. Time-resolved analysis was conducted to optimize the gate delay and gate width for the detection of the C I emission line at 247.9 nm to monitor the epoxy resin matrix of CFRP composites and the Si I emission line at 288.2 nm for detection of silicone contaminants in CFRP. To study the surface sensitivity to silicone contamination, CFRP surfaces were coated with polydimethylsiloxane (PDMS), the active ingredient in many mold release agents. The presence of PDMS was studied by inspecting the Si I emission lines at 251.6 nm and 288.2 nm. The measured PDMS areal densities ranged from 0.15 to 2 μg/cm(sup 2). LIBS measurements were performed before and after laser surface ablation. The results demonstrate the successful detection of PDMS thin layers on CFRP using picosecond μLIBS.

Rodolfo Ledesma↗

Surface Bacterial-Spore Assay Using Tb3+/DPA Luminescence

Equipment and a method for rapidly assaying solid surfaces for contamination by bacterial spores are undergoing development. The method would yield a total (nonviable plus viable) spore count of a surface within minutes and a viable-spore count in about one hour. In this method, spores would be collected from a surface by use of a transparent polymeric tape coated on one side with a polymeric adhesive that would be permeated with one or more reagent(s) for detection of spores by use of visible luminescence. The sticky side of the tape would be pressed against a surface to be assayed, then the tape with captured spores would be placed in a reader that illuminates the sample with ultraviolet light and counts the green luminescence spots under a microscope to quantify the number of bacterial spores per unit area. The visible luminescence spots seen through the microscope would be counted to determine the concentration of spores on the surface. This method is based on the chemical and physical principles of methods described in several prior NASA Tech Briefs articles, including Live/Dead Spore Assay Using DPA-Triggered Tb Luminescence (NPO-30444), Vol. 27, No. 3 (March 2003), page 7a. To recapitulate: The basic idea is to exploit the observations that (1) dipicolinic acid (DPA) is present naturally only in bacterial spores; and (2) when bound to Tb3+ ions, DPA triggers intense green luminescence of the ions under ultraviolet excitation; (3) DPA can be released from the viable spores by using L-alanine to make them germinate; and (4) by autoclaving, microwaving, or sonicating the sample, one can cause all the spores (non-viable as well as viable) to release their DPA. One candidate material for use as the adhesive in the present method is polydimethysiloxane (PDMS). In one variant of the method for obtaining counts of all (viable and nonviable) spores the PDMS would be doped with TbCl3. After collection of a sample, the spores immobilized on the sticky tape surface would be lysed by heating or microwaving to release their DPA. Tb3+ ions from the TbCl3 would become bound to the released DPA. The tape would then be irradiated with ultraviolet and examined as described above. In another variant of the method - for obtaining counts of viable spores only - the PDMS would be doped with L-alanine in addition to TbCl3. As now envisioned, a fully developed apparatus for implementing this method would include a pulsed source of ultraviolet light and a time-gated electronic camera to record the images seen through the microscope during a prescribed exposure interval at a prescribed short time after an ultraviolet pulse. As in the method of the second-mentioned prior article, the pulsing and time-gating would be used to discriminate between the longer-lived Tb3+/DPA luminescence and the shorter-lived background luminescence in the same wavelength range. In a time-gated image, the bright luminescence from bacterial spores could easily be seen against a dark background.

Ponce, Adrian↗

Organosiloxane working fluids for the liquid droplet radiator

Siloxane-based working fluids for advanced space radiators requiring direct fluid exposure to the space environment are evaluated. Isolation of five candidate fluids by vacuum distillation from existing siloxane polymers is discussed. The five fluids recovered include a polydimethylsiloxane, three phenyl-containing siloxanes, and a methylhexylsiloxane. Vapor pressures and viscosities for the five fluids are reported over the temperature range of 250 to 400 K. Use of thermal-gravimetric analysis to reliably estimate vapor pressures of 10 to the -8 power Pascals is described. Polydimethylsiloxane (PDMS) and polymethylphenylsiloxane (PMPS) are selected from the five candidate fluids based on favorable vapor pressure and viscosity, as well as perceived stability in low-Earth orbit environments. Characterization of these fluids by infrared spectroscopy, Si-29 NMR, gel-permeation chromatography, and liquid chromatography is presented. Both fluids consist of narrow molecular weight distributions, with average molecular weights of about 2500 for PDMS and 1300 for PMPS.

Buch, R. R.↗

CO2 Acquisition Membrane (CAM)

The objective of CAM is to develop, test, and analyze thin film membrane materials for separation and purification of carbon dioxide (CO2) from mixtures of gases, such as those found in the Martian atmosphere. The membranes are targeted toward In Situ Resource Utilization (ISRU) applications that will operate in extraterrestrial environments and support future unmanned and human space missions. A primary application is the Sabatier Electrolysis process that uses Mars atmosphere CO2 as raw material for producing water, oxygen, and methane for rocket fuel and habitat support. Other applications include use as an inlet filter to collect and concentrate Mars atmospheric argon and nitrogen gases for habitat pressurization, and to remove CO2 from breathing gases in Closed Environment Life Support Systems (CELSS). CAM membrane materials include crystalline faujasite (FAU) zeolite and rubbery polymers such as silicone rubber (PDMS) that have been shown in the literature and via molecular simulation to favor adsorption and permeation of CO2 over nitrogen and argon. Pure gas permeation tests using commercial PDMS membranes have shown that both CO2 permeance and the separation factor relative to other gases increase as the temperature decreases, and low (Delta)P(Sub CO2) favors higher separation factors. The ideal CO2/N2 separation factor increases from 7.5 to 17.5 as temperature decreases from 22 C to -30 C. For gas mixtures containing CO2, N2, and Ar, plasticization decreased the separation factors from 4.5 to 6 over the same temperature range. We currently synthesize and test our own Na(+) FAU zeolite membranes using standard formulations and secondary growth methods on porous alumina. Preliminary tests with a Na(+) FAU membrane at 22 C show a He/SF6 ideal separation factor of 62, exceeding the Knudsen diffusion selectivity by an order of magnitude. This shows that the membrane is relatively free from large defects and associated non-selective (viscous flow) transport mechanisms. The Membrane Test Facility (MTF) has been developed to measure membrane permeance over a wide range of temperature and pressure. The facility uses two volume compartments separated by the membrane that are instrumented to measure temperature, delta pressure across the membrane, and gas composition. A thermal shroud supports and encloses the membrane, and provides temperature control. Methods were developed to determine membrane permeance using the first order decay of the pressure difference between the sealed compartments, using the total pressure for pure gases, and partial pressure of each species in gas mixtures. The technique provides an end-to-end measurement of gas permeance that includes concentration polarization effects. Experiments have shown that in addition to membrane permeance properties, the geometry and design of associated structures play an important role in how membrane systems will function on Mars.

Mason, Larry W.↗

Dielectric relaxation behavior of poly(acrylonitri1e-co-methacrylonitrile) microcapsules dispersed in a silicone matrix

The dielectric relaxation behavior of poly(acry1onitrile-co-methacrylonitrile) dispersed in a cured polydimethyl siloxane (PDMS) matrix as microcapsules was investigated over multiple thermal cycles and at varying concentrations. The copolymer microcapsules contained an isopentane core. In the PDMS matrix this copolymer displayed a pronounced relaxation signal at temperatures above the glass transition of the copolymers due to Maxwell-Wagner-Sillars (MWS) relaxation. The mechanism of MWS relaxation interpreted by the Havriliak-Negami and Kohlrausch-Williams-Watts relaxation functions was found to be very similar to previous studies of neat polyacrylonitrile and its copolymer. The activation energy of the relaxation decreased over successive thermal cycling coincident with a decreasing strength of the relaxation. These observations were attributed to the decreasing concentration of nitrile groups due to intramolecular cyclizations.

Park, Taigyoo↗

Dielectric Relaxation Behavior of Poly(acrylonitrile-co-methacrylonitrile) Microcapsules Dispersed in a Silicone Matrix

The dielectric relaxation behavior of poly(acrylonitrile-co-methacrylonitrile) dispersed in a cured polydimethyl siloxane (PDMS) matrix as microcapsules was investigated over multiple thermal cycles and at varying concentrations. The copolymer microcapsules contained an isopentane core. In the PDMS matrix this copolymer displayed a pronounced relaxation signal at temperatures above the glass transition of the copolymers due to Maxwell-Wagner-Sillars (MWS) relaxation. The mechanism of MWS relaxation interpreted by the Havriliak-Negami and Kohlrausch-Williams-Watts relaxation functions was found to be very similar to previous studies of neat polyacrylonitrile and its copolymer. The activation energy of the relaxation decreased over successive thermal cycling coincident with a decreasing strength of the relaxation. These observations were attributed to the decreasing concentration of nitrile groups due to intramolecular cyclizations.

Park, Taigyoo↗

Fabricating PFPE Membranes for Microfluidic Valves and Pumps

A process has been developed for fabricating membranes of a perfluoropolyether (PFPE) and integrating them into valves and pumps in laboratory-on-achip microfluidic devices. Membranes of poly(tetrafluoroethylene) [PTFE] and poly(dimethylsilane) [PDMS] have been considered for this purpose and found wanting. By making it possible to use PFPE instead of PTFE or PDMS, the present process expands the array of options for further development of microfluidic devices for diverse applications that could include detection of biochemicals of interest, detection of toxins and biowarfare agents, synthesis and analysis of proteins, medical diagnosis, and synthesis of fuels.

Greer, Frank↗

Silicone-Rubber Microvalves Actuated by Paraffin

Microvalves containing silicone-rubber seals actuated by heating and cooling of paraffin have been proposed for development as integral components of microfluidic systems. In comparison with other microvalves actuated by various means (electrostatic, electromagnetic, piezoelectric, pneumatic, and others), the proposed valves (1) would contain simpler structures that could be fabricated at lower cost and (2) could be actuated by simpler (and thus less expensive) control systems. Each valve according to the proposal would include a flow channel bounded on one side by a flat surface and on the other side by a curved surface defined by an arched-cross-section, elastic seal made of silicone rubber [polydimethylsilane (PDMS)]. The seal would be sized and shaped so that the elasticity of the PDMS would hold the channel open except when the seal was pressed down onto the flat surface to close the channel. The principle of actuation would exploit the fact that upon melting or freezing, the volume of a typical paraffin increases or decreases, respectively, by about 15 percent. In a valve according to the proposal, the seal face opposite that of the channel would be in contact with a piston-like plug of paraffin. In the case of a valve designed to be normally open at ambient temperature, one would use a paraffin having a melting temperature above ambient. The seal would be pushed against the flat surface to close the channel by heating the paraffin above its melting temperature. In the case of a valve designed to be normally closed at ambient temperature, one would use a paraffin having a melting temperature below ambient. The seal would be allowed to spring away from the flat surface to open the channel by cooling the paraffin below its melting temperature. The availability of paraffins that have melting temperatures from 70 to +80 C should make it possible to develop a variety of normally closed and normally open valves. The figure depicts examples of prototype normally open and normally closed valves according to the proposal. In each valve, an arch cross section defining a channel having dimensions of the order of tens of micrometers would be formed in a silicone-rubber sheet about 40 m thick. The silicone rubber sheet would be hermetically sealed to a lower glass plate that would define the sealing surface and to an upper glass plate containing a well. The well would be filled with paraffin and capped with a rigid restraining layer of epoxy. In the normally open valve, the paraffin would have a melting temperature above ambient (e.g., 40 C) and the wall of the well would be coated with a layer of titanium that would serve as an electric heater. In the normally closed valve, the paraffin would have a melting temperature below ambient (e.g.-5 C). Instead of a heater in the well, the normally closed valve would include a thermoelectric cooler on top of the epoxy cap.

Svelha, Danielle↗

Design and Delivery of a Filter for Removal of Siloxanes from the ISS Atmosphere

Dimethylsilanediol (DMSD) has been identified as a problematic chemical contaminant aboard ISS. This contaminant was initially identified in the ISS condensate and in the Water Processor Assembly (WPA) product water in 2010 when an increasing total organic carbon (TOC) trend was detected in the water produced by the WPA. DMSD is not a crew health hazard at the levels observed in the product water, but it may degrade the performance of the Oxygen Generation System (OGS) which uses product produced by the WPA for electrolysis. In addition, DMSD can prevent the effective operation of the WPA catalytic reactor, and necessitates early replacement of Multifiltration Beds in the WPA. An investigation into the source of DMSD has determined that polydimethylsiloxanes (PDMSs) are hydrolyzing in the Condensing Heat Exchanger (CHX) to form DMSD. PDMSs are prevalent aboard ISS from a variety of sources, including crew hygiene products, adhesives, caulks, lubricants, and various nonmetallics. TPDMSs are also implicated in CHX hydrophilic coating degradation, rendering it hydrophobic and adversely affecting its ability to effectively transmit water to the condensate bus. Eventually this loss in performance results in water droplets in the air flow out of the CHX core, which can lead to microbial growth in the air ducts and can impact the performance of downstream systems. Design concepts have now been developed for removing PDMS in the air stream before it can reach the CHX core, thus preventing degradation of the coating and decomposition of the PDMS to DMSD. This paper summarizes the current status of the effort to deliver filters to ISS for removing PDMSs from the atmosphere before they can adversely impact the performance of the CHX coating and the WPA.

Carter, Layne↗