In the new study led by Rice graduate students Lauren Taylor and Oliver Dewey, the researchers noted that wet-spun carbon nanotube fibres, which could lead to breakthroughs in a host of medical and materials applications, have doubled in strength and conductivity every three years, a trend that spans almost two decades.

While that may never mimic Moore’s Law, which set a benchmark for computer chip advances for decades, Pasquali and his team are doing their part to advance the method they pioneered to make carbon nanotube fibres.

The lab’s threadlike fibres, with tens of millions of nanotubes in cross-section, are being studied for use as bridges to repair damaged hearts, as electrical interfaces with the brain, for use in cochlear implants, as flexible antennas and for automotive and aerospace applications.

They are also part of the Carbon Hub, a multi-university research initiative launched in 2019 by Rice with support from Shell, Prysmian and Mitsubishi to create a zero-emissions future.

“Carbon nanotube fibres have long been touted for their potential superior properties,” Pasquali said. “Two decades of research at Rice and elsewhere have made this potential a reality. Now we need a worldwide effort to increase production efficiency so these materials could be made with zero carbon dioxide emissions and potentially with concurrent production of clean hydrogen.”

“The goal of this paper is to put forth the record properties of the fibres produced in our lab,” Taylor said. “These improvements mean we’re now surpassing Kevlar in terms of strength, which for us is a really big achievement. With just another doubling, we would surpass the strongest fibres on the market.”

The flexible Rice fibres have a tensile strength of 4.2 gigapascals (GPa), compared to 3.6 GPa for Kevlar fibres. The fibres require long nanotubes with high crystallinity; that is, regular arrays of carbon-atom rings with few defects. The acidic solution used in the Rice process also helps reduce impurities that can interfere with fibre strength and enhance the nanotubes’ metallic properties through residual doping, Dewey said.

“The length, or aspect ratio, of the nanotubes, is the defining characteristic that drives the properties in our fibres,” he said, noting the surface area of the 12-micrometre nanotubes used in Rice fibre facilitates better van der Waals bonds. “It also helps that the collaborators who grow our nanotubes optimise for solution processing by controlling the number of metallic impurities from the catalyst and what we call amorphous carbon impurities.”

The researchers said the fibres’ conductivity has improved to 10.9 megasiemens (million siemens) per meter. “This is the first time a carbon nanotube fibre has passed the 10 megasiemens threshold, so we’ve achieved a new order of magnitude for nanotube fibres,” Dewey said. Normalised for weight, he said the Rice fibres achieve about 80% of the conductivity of copper.

“But we’re surpassing platinum wire, which is a big achievement for us,” Taylor said, “and the fibre thermal conductivity is better than any metal and any synthetic fibres, except for pitch graphite fibres.”

The lab’s goal is to make the production of superior fibres efficient and inexpensive enough to be incorporated by industry on a large scale, Dewey said. Solution processing is common in the production of other kinds of fibres, including Kevlar, so factories could use familiar processes without major retooling.

“The benefit of our method is that it’s essentially plug-and-play,” he said. “It’s inherently scalable and fits in with the way synthetic fibre are already made.”

“There’s a notion that carbon nanotubes are never going to be able to obtain all the properties that people have been hyping now for decades,” Taylor said. “But we’re making good gains year over year. It’s not easy, but we still do believe this technology is going to change the world.”

Co-authors of the paper are Rice alumnus Robert Headrick; graduate students Natsumi Komatsu and Nicolas Marquez Peraca; Geoff Wehmeyer, an assistant professor of mechanical engineering; and Junichiro Kono, the Karl F. Hasselmann Professor in Engineering and a professor of electrical and computer engineering, of physics and astronomy, and of materials science and nanoengineering. Pasquali is the A.J. Hartsook Professor of Chemical and Biomolecular Engineering, of chemistry and of materials science and nanoengineering.

The U.S. Air Force Office of Scientific Research, the Robert A. Welch Foundation, the Department of Energy’s Advanced Manufacturing Office and the Advanced Research Projects Agency-Energy supported the research.

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In a new study, Texas A&M University researchers have used a natural plant product, called cellulose nanocrystals, to pin and coat carbon nanotubes uniformly onto the carbon-fibre composites. The researchers said their prescribed method is quicker than conventional methods and also allows the designing of carbon-fibre composites from the nanoscale.

Composites are built in layers. For example, polymer composites are made of layers of fibre, like carbon fibres or Kevlar, and a polymer matrix. This layered structure is the source of the composites’ weakness. Any damage to the layers causes fractures, a process technically known as delamination.

To increase strength and give carbon-fibre composites other desirable qualities, such as electrical and thermal conductivity, carbon nanotubes are often added. However, the chemical processes used for incorporating the carbon nanotubes into these composites often cause the nanoparticles to clump up, reducing the overall benefit of adding these particles.

“The problem with nanoparticles is similar to what happens when you add coarse coffee powder to milk—the powder agglomerates or sticks to each other,” said Dr Amir Asadi, assistant professor in the Department of Engineering Technology and Industrial Distribution. “To fully take advantage of the carbon nanotubes, they need to be separated from each other first, and then somehow designed to go to a particular location within the carbon-fibre composite.”

To facilitate the even distribution of carbon nanotubes, Asadi and his team turned to cellulose nanocrystals, a compound easily obtained from recycled wood pulp. These nanocrystals have segments on their molecules that attract water and other segments that get repelled by water. This unique molecular structure offers the ideal solution to construct composites at the nanoscale, said Asadi.

The hydrophobic part of the cellulose nanocrystals binds to the carbon fibres and anchors them onto the polymer matrix. On the other hand, the water-attractive portions of the nanocrystals help in dispersing the carbon fibres evenly, much like how sugar, which is hydrophilic, dissolves in water uniformly rather than clumping and settling to the bottom of a cup.

For their experiments, the researchers used a commercially available carbon-fibre cloth. To this cloth, they added an aqueous solution of cellulose nanocrystals and carbon nanotubes and then applied strong vibration to mix all of the items together. Finally, they left the material to dry and spread resin on it to gradually form the carbon nanotube coated polymer composite.

Upon examining a sample of the composite using electron microscopy, Asadi and his team observed that the cellulose nanocrystals attached to the tips of the carbon nanotubes, orienting the nanotubes in the same direction. They also found that cellulose nanocrystals increased the composite’s resistance to bending by 33% and its inter-laminar strength by 40% based on measuring the mechanical properties of the material under extreme loading.

“In this study, we have taken the approach of designing the composites from the nanoscale using cellulose nanocrystals. This method has allowed us to have more control over the polymer composites’ properties that emerge at the macroscale,” said Asadi. “We think that our technique is a path forward in scaling up the processing of hybrid composites, which will be useful for a variety of industries, including airline and automobile manufacturing.”

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Now MIT engineers have developed a method to produce aerospace-grade composites without the enormous ovens and pressure vessels. The technique may help to speed up the manufacturing of aeroplanes and other large, high-performance composite structures, such as blades for wind turbines.

The researchers detail their new method in a paper published in the journal Advanced Materials Interfaces.

If you’re making a primary structure like a fuselage or wing, you need to build a pressure vessel, or autoclave, the size of a two- or three-story building, which itself requires time and money to pressurize. These things are massive pieces of infrastructure. Now we can make primary structure materials without autoclave pressure, so we can get rid of all that infrastructure. Brian Wardle, professor of aeronautics and astronautics at MIT

Wardle’s co-authors on the paper are lead author and MIT postdoc Jeonyoon Lee, and Seth Kessler of Metis Design Corporation, an aerospace structural health monitoring company based in Boston.

Out of the oven, into a blanket

In 2015, Lee led the team, along with another member of Wardle’s lab, in creating a method to make aerospace-grade composites without requiring an oven to fuse the materials together. Instead of placing layers of material inside an oven to cure, the researchers essentially wrapped them in an ultrathin film of carbon nanotubes (CNTs). When they applied an electric current to the film, the CNTs, like a nanoscale electric blanket, quickly generated heat, causing the materials within to cure and fuse together.

With this out-of-oven, or OoO, technique, the team was able to produce composites as strong as the materials made in conventional aeroplane manufacturing ovens, using only 1 per cent of the energy.

The researchers next looked for ways to make high-performance composites without the use of large, high-pressure autoclaves — building-sized vessels that generate high enough pressures to press materials together, squeezing out any voids, or air pockets, at their interface.

Researchers including Wardle’s group have explored “out-of-autoclave,” or OoA, techniques to manufacture composites without using the huge machines. But most of these techniques have produced composites where nearly 1 per cent of the material contains voids, which can compromise a material’s strength and lifetime. In comparison, aerospace-grade composites made in autoclaves are of such high quality that any voids they contain are negligible and not easily measured.

Straw pressure

Part of Wardle’s work focuses on developing nanoporous networks — ultrathin films made from aligned, microscopic material such as carbon nanotubes, that can be engineered with exceptional properties, including colour, strength, and electrical capacity. The researchers wondered whether these nanoporous films could be used in place of giant autoclaves to squeeze out voids between two material layers, as unlikely as that may seem.

A thin film of carbon nanotubes is somewhat like a dense forest of trees, and the spaces between the trees can function like thin nanoscale tubes or capillaries. A capillary such as a straw can generate pressure based on its geometry and its surface energy, or the material’s ability to attract liquids or other materials.

The researchers tested their idea in the lab by growing films of vertically aligned carbon nanotubes using a technique they previously developed, then laying the films between layers of materials that are typically used in the autoclave-based manufacturing of primary aircraft structures. They wrapped the layers in a second film of carbon nanotubes, which they applied an electric current to heat it up. They observed that as the materials heated and softened in response, they were pulled into the capillaries of the intermediate CNT film.

The resulting composite lacked voids, similar to aerospace-grade composites that are produced in an autoclave. The researchers subjected the composites to strength tests, attempting to push the layers apart, the idea being that voids, if present, would allow the layers to separate more easily.

The team will next look for ways to scale up the pressure-generating CNT film. In their experiments, they worked with samples measuring several centimetres wide — large enough to demonstrate that nanoporous networks can pressurize materials and prevent voids from forming. To make this process viable for manufacturing entire wings and fuselages, researchers will have to find ways to manufacture CNT and other nanoporous films at a much larger scale.

He plans also to explore different formulations of nanoporous films, engineering capillaries of varying surface energies and geometries, to be able to pressurize and bond other high-performance materials.

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The team are using carbon nanotubes, which are linked hexagons of carbon atoms in the shape of a cylinder, to build the heat shields. Sheets of those nanotubes are also known as “buckypaper,” a material with incredible abilities to conduct heat and electricity that has been a focus of study at HPMI. By soaking the buckypaper in a resin made of a compound called phenol, the researchers were able to create a lightweight, flexible material that is also durable enough to potentially protect the body of a rocket or jet from the intense heat it faces while flying.

Existing heat shields are often very thick compared to the base they protect, said Ayou Hao, a research faculty member at HPMI. This design lets engineers build a very thin shield, like a sort of skin that protects the aircraft and helps support its structure.

After building heat shields of varying thicknesses, the researchers put them through a series of tests including applying a flame to see how they prevented heat from reaching the carbon fibre layer they were meant to protect. After that, the researchers bent the samples to see how strong they remained.

They found the samples with sheets of buckypaper were better than control samples at dispersing heat and keeping it from reaching the base layer. They also stayed strong and flexible compared to control samples made without protective layers of nanotubes.

That flexibility is a helpful quality. The nanotubes are less vulnerable to cracking at high temperatures compared to ceramics, a typical heat shield material. They’re also lightweight, which is helpful for engineers who want to reduce the weight of anything on an aircraft that doesn’t help the way it flies.

The project received second place among peer-reviewed posters at the 2019 National Space and Missile Materials Symposium and received a third place at the Society for the Advancement of Material and Process Engineering 2019 University Research Symposium.

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This material is the first key component of futuristic smart uniforms that also will respond to and protect from environmental chemical hazards.

High breathability is a critical requirement for protective clothing to prevent heat-stress and exhaustion when military personnel are engaged in missions in contaminated environments. Current protective military uniforms are based on heavyweight full-barrier protection or permeable adsorptive protective garments that cannot meet the critical demand of simultaneous high comfort and protection, and provide a passive rather than active response to an environmental threat.

The LLNL team fabricated flexible polymeric membranes with aligned carbon nanotube (CNT) channels as moisture conductive pores. The size of these pores (less than 5 nanometers, nm) is 5,000 times smaller than the width of a human hair.

Ngoc Bui, the lead author of the paper said;

We demonstrated that these membranes provide rates of water vapour transport that surpass those of commercial breathable fabrics like GoreTex, even though the CNT pores are only a few nanometers wide.

To provide high breathability, the new composite material takes advantage of the unique transport properties of carbon nanotube pores. By quantifying the membrane permeability to water vapour, the team found for the first time that, when a concentration gradient is used as a driving force, CNT nano-channels can sustain gas-transport rates exceeding that of a well-known diffusion theory by more than one order of magnitude.

These membranes also provide protection from biological agents due to their very small pore size – less than 5 nanometers (nm) wide. Biological threats like bacteria or viruses are much larger and typically more than 10-nm in size. Performed tests demonstrated that the CNT membranes repelled Dengue virus from aqueous solutions during filtration tests. This confirms that LLNL-developed CNT membranes provide effective protection from biological threats by size exclusion rather than by merely preventing wetting.

Furthermore, the results show that CNT pores combine high breathability and bio-protection in a single functional material.

However, chemical agents are much smaller in size and require the membrane pores to be able to react to block the threat. To encode the membrane with a smart and dynamic response to small chemical hazards, LLNL scientists and collaborators are surface modifying these prototype carbon nanotube membranes with chemical-threat-responsive functional groups. These functional groups will sense and block the threat like gatekeepers on the pore entrance. A second response scheme also is in development – similar to how living skin peels off when challenged with dangerous external factors. The fabric will exfoliate upon reaction with the chemical agent.

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NASA’s CubeSat Launch initiative (CSLI) provides opportunities for small satellite payloads to fly on rockets planned for upcoming launches. These CubeSats are flown as auxiliary payloads on previously planned missions.

Small satellites are playing an increasingly larger role in exploration, technology demonstration, scientific research and educational investigations at NASA. These miniature satellites provide a low-cost platform for NASA missions, including planetary space exploration. They also allow an inexpensive means to engage students in all phases of satellite development, operation and exploitation through real-world, hands-on research and development experience on NASA-funded ride share launch opportunities.

The first ever carbon-nanotube resin mirror could prove central to creating a low-cost space telescope for a range of CubeSat scientific investigations.

Unlike most telescope mirrors made of glass or aluminium, this particular optic is made of carbon nanotubes embedded in an epoxy resin. Sub-micron-size, cylindrically shaped, carbon nanotubes exhibit extraordinary strength and unique electrical properties, and are efficient conductors of heat. Owing to these unusual properties, the material is valuable to nanotechnology, electronics, optics, and other fields of materials science, and, as a consequence, are being used as additives in various structural materials.

The use of a carbon-nanotube optic in a CubeSat telescope offers a number of advantages. In addition to being lightweight, highly stable, and easily reproducible, carbon-nanotube mirrors do not require polishing — a time-consuming and often times expensive process typically required to assure a smooth, perfectly shaped mirror.

To make a mirror, technicians simply pour the mixture of epoxy and carbon nanotubes into a mandrel or mould fashioned to meet a particular optical prescription. They then heat the mould to cure and harden the epoxy. Once set, the mirror then is coated with a reflective material of aluminium and silicon dioxide.

Many of the mirror segments in these telescopes are identical and can therefore be produced using a single mandrel. Carbon-nanotube mirrors can also be made into ‘smart optics’. To maintain a single perfect focus in the Keck telescopes, for example, each mirror segment has several externally mounted actuators that deform the mirrors into the specific shapes required at different telescope orientations.

This technology can potentially enable very large-area technically active optics in space, and can address everything from astronomy and Earth observing to deep-space communications.

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Engineers at MIT have now developed a carbon nanotube (CNT) film that can heat and solidify a composite without the need for massive ovens. When connected to an electrical power source, and wrapped over a multilayer polymer composite, the heated film stimulates the polymer to solidify.

The group tested the film on a common carbon fibre material used in aircraft components, and found that the film created a composite as strong as that manufactured in conventional ovens — while using only 1% of the energy.

Brian L. Wardle, an associate professor of aeronautics and astronautics at MIT said;

Typically, if you’re going to cook a fuselage for an Airbus A350 or Boeing 787, you’ve got about a four-story oven that’s tens of millions of dollars in infrastructure that you don’t need. Our technique puts the heat where it is needed, in direct contact with the part being assembled. Think of it as a self-heating pizza. … Instead of an oven, you just plug the pizza into the wall and it cooks itself.

The carbon nanotube film is also incredibly lightweight: After it has fused the underlying polymer layers, the film itself — a fraction of a human hair’s diameter — meshes with the composite, adding negligible weight. The team, including MIT graduate students Jeonyoon Lee and Itai Stein and Seth Kessler of the Metis Design Corporation, has published its results in the journal ACS Applied Materials and Interfaces.

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Wardle and his colleagues have experimented with CNT films in recent years, mainly for deicing airplane wings. The team recognised that in addition to their negligible weight, carbon nanotubes heat efficiently when exposed to an electric current.

The research team first developed a technique to create a film of aligned carbon nanotubes composed of tiny tubes of crystalline carbon, standing upright like trees in a forest. The researchers used a rod to roll the “forest” flat, creating a dense film of aligned carbon nanotubes. In experiments, they integrated the film into airplane wings via conventional, oven-based curing methods, showing that when voltage was applied, the film generated heat, preventing ice from forming.

So how hot can you go? In initial experiments, the researchers investigated the film’s potential to fuse two types of aerospace-grade composite typically used in aircraft wings and fuselages. Normally the material, composed of about 16 layers, is solidified, or cross-linked, in a high-temperature industrial oven.

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The researchers manufactured a CNT film about the size of a Post-It note, and placed the film over a square of Cycom 5320–1. They connected electrodes to the film, then applied a current to heat both the film and the underlying polymer in the Cycom composite layers.

They then measured the energy required to solidify, or cross-link, the polymer and carbon fibre layers, finding that the CNT film used one-hundredth the electricity required for traditional oven-based methods to cure the composite. Both methods generated composites with similar properties, such as cross-linking density.

The results pushed the group to test the CNT film further: As different composites require different temperatures in order to fuse, the researchers looked to see whether the CNT film could, quite literally, take the heat.

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To do this, they tested the film’s ability to generate higher and higher temperatures, and found it topped out at over 1,000 F. In comparison, some of the highest-temperature aerospace polymers require temperatures up to 750 F in order to solidify.

The team is working with industrial partners to find ways to scale up the technology to manufacture composites large enough to make airplane fuselages and wings. The group’s carbon nanotube film may go toward improving the quality and efficiency of fabrication processes for large composites, such as wings on commercial aircraft. The new technique may also open the door to smaller firms that lack access to large industrial ovens.

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Inspired by the way living organisms have evolved in nature to perform complex tasks with remarkable ease, a group of researchers from Durham University in the UK and the University of São Paulo-USP in Brazil is exploring similar “evolutionary” methods to create information processing devices.

In the Journal of Applied Physics, the group describes using single-walled carbon nanotube composites as a material in “unconventional” computing. By studying the mechanical and electrical properties of the materials, they discovered a correlation between the Nanotubes’ concentration, viscosity, conductivity and the computational capability of the composite.

Mark K. Massey, research associate, School of Engineering and Computing Sciences at Durham University said;

Instead of creating circuits from arrays of discrete components (transistors in digital electronics), our work takes a random disordered material and then ‘trains’ the material to produce a desired output.

This emerging field of research is known as “evolution-in-materio,” a term coined by Julian Miller at the University of York in the UK What exactly is it? An interdisciplinary field blends together materials science, engineering and computer science. Although still in its early stages, the concept has already shown that by using an approach similar to natural evolution, materials can be trained to mimic electronic circuits–without needing to design the material structure in a specific way.

“The material they are a mixture of carbon nanotubes and polymer, which creates a complex electrical structure. When voltages (stimuli) are applied at points of the material, its electrical properties change. When the correct signals are applied to the material, it can be trained or ‘evolved’ to perform a useful function.”

While the group doesn’t expect to see their method compete with high-speed silicon computers, it could turn out to be a complementary technology. And with more research, it could lead to new techniques for making electronics devices. The approach may find applications within the realm of “analog signal processing or low-power, low-cost devices in the future.

The next stage of the group’s research will be to investigate evolving devices as part of the material fabrication “hardware-in-the-loop” evolution. “This exciting approach could lead to further enhancements in the field of evolvable electronics,” said Massey.

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New experiments show that the biocompatible fibres are ideal candidates for small, safe electrodes that interact with the brain’s neuronal system, and could replace much larger electrodes currently used in devices for deep brain stimulation therapies in Parkinson’s disease patients.

They could also advance technologies to restore sensory or motor functions and brain-machine interfaces as well as deep brain stimulation therapies for other neurological disorders, including dystonia and depression, the researchers wrote.

The fibres are made from bundles of long nanotubes originally intended for aerospace applications where strength, weight and conductivity are paramount. The individual nanotubes measure only a few nanometers across, but when millions are bundled in a process called wet spinning, they become thread-like fibres about a quarter the width of a human hair.

Matteo Pasquali said on the creation of the fibres;

We developed these fibres as high-strength, high-conductivity materials. Yet, once we had them in our hand, we realised that they had an unexpected property: They are really soft, much like a thread of silk. Their unique combination of strength, conductivity and softness makes them ideal for interfacing with the electrical function of the human body.

Intensive testing on cells and then in rats with Parkinson’s symptoms proved the fibres are stable and as efficient as commercial platinum electrodes at only a fraction of the size. The soft fibres caused little inflammation, which helped maintain strong electrical connections to neurons by preventing the body’s defences from scarring and encapsulating the site of the injury.

Doctors who implant deep brain stimulation devices start with a recording probe able to “listen” to neurons that emit characteristic signals depending on their functions, once a surgeon finds the right spot, the probe is removed and the stimulating electrode gently inserted. Rice carbon nanotube fibres that send and receive signals would simplify implantation.

The fibres could one day lead to self-regulating therapeutic devices for Parkinson’s and other patients. Current devices include an implant that sends electrical signals to the brain to calm the tremors that afflict Parkinson’s patients.

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The scientists used bundled carbon nanotubes to incubate a type of white blood cell that is important to immune system functions. According to the researchers, the topography of the nanotubes enhances interactions between cells and long-term cultures, providing a fast and effective stimulation of the cytotoxic T cells that are important for eradicating cancer.

The team at Yale modified the nanotubes by chemically binding them to polymer nanoparticles that held a particular cell signaling protein that encourages T cell growth and proliferation. In order to mimic the body’s methods for stimulating cytotoxic T cell proliferation, the scientists seeded the surfaces of the carbon nanotubes with molecules that signaled which of the patient’s cells were foreign or toxic and should be attacked.

Over the course of 14 days, the number of T cells cultured on the composite nanosystem expanded by a factor of 200, Tarek Fahmy, an associate professor of biomedical engineering and the study’s principal investigator said;

In repressing the body’s immune response, tumours are like a castle with a moat around it, our method recruits significantly more cells to the battle and arms them to become super-killers.

According to Fahmy, previous procedures for boosting antigen-specific T cells required exposing the patient’s harvested immune cells to other cells that stimulate activation and proliferation, a costly procedure that risks an adverse reaction to foreign cells. The Yale team’s use of magnetic CNT-polymer composites eliminates that risk by using simple, inexpensive magnets to separate the composites from the T cells prior to injection.

Modulatory nanotechnologies can present unique opportunities for promising new therapies such as T cell immunotherapy, engineers are progressing toward the design of the next generations of nanomaterials, allowing for further breakthrough in many fields, including cancer research.

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