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HXN team members, from left, Evgeny Nazaretski, Ken Lauer, Sebastian Kalbfleisch, Xiaojing Huang, Yong Chu, Nathalie Bouet and Hanfei Yan. Photo courtesy of BNL

By Daniel Dunaief

There’s precision in measurements and then there’s the world of Yong Chu. The head of a beamline that’s housed off to the side in a separate, concrete structure from similar efforts at Brookhaven National Laboratory, Chu led the design, construction and commissioning of a sophisticated beamline with a resolution of as low as 3 nanometers, which he hopes will get down to 1 nanometer within a year.

Just as a measure of contrast, a human hair is about 80,000 nanometers wide. Why so fine a resolution? For starters, seeing objects or processes at that high level can offer insights into how they function, how to improve their manufacture or how to counteract the effects of harmful processes.

With a battery, for example, the Hard X-ray Nanoprobe, or HXN beamline, could help reveal structural weaknesses in the nanostructure that could cause safety issues. In biology, numerous functions involve sub-cellular organelles that respond to proteins. Proteins are typically smaller than the HXN beamline can image, although researchers can tag the proteins with metals, which allows Chu, his colleagues and visiting scientists to see an aggregate of these proteins.

The HXN beamline can also help explore environmental problems, such as how plants transport harmful nanoparticles to their fruits or how artificial compounds absorb nuclear waste. Imaging beamlines that use micro-focused beams typically offer spatial resolution of 10 microns, 1 micron or even 100 nanometers, according to Ryan Tappero, the head scientist at the X-ray Fluorescence Microprobe at BNL, who has used the HXN for his research. Using the NSLS II source properties and a new x-ray optics development routinely offers resolution of 10 nanometers, which pushes the spatial resolution down by another factor of 10, which makes the HXN, according to Tappero, a “game changer.”

Tappero described Chu as a “rock star” and suggested he was an “exceptional beamline scientist” who is “very knowledgeable about X-ray optics.”

BNL houses 19 beamlines at the National Synchrotron Light Source II, a state-of-the-art facility large enough that scientists ride adult tricycles inside it to travel from one beamline to another and to transport supplies around the facility. BNL is building another nine beamlines that it hopes to have operational within the next 18 months. Each of these beamlines offers a different way to explore the world of matter. Some beamlines do not use a focused beam, while others produce beams with high angular or high energy resolution. Imaging beamlines such as the HXN produce a small beam size.

The HXN beamline has the highest spatial resolution of any beamline at the NSLS-II. Scientists building the HXN grew a nanofocusing lens with a dedicated deposition system that was constructed at the NSLS-II Research and Development lab. The system grew a nanofocusing lens a layer at a time, alternating materials and controlling the thickness at better than 1 nanometer, Chu explained.

The beamline where Chu works has padded walls, a door separating it from the rest of the light source and a monitor that records the temperature to the thousandths of a degree. “We are constantly monitoring the temperature around the X-ray microscope and inside of the X-ray microscope chamber,” he said. Around the microscope, he can keep the temperature stable within 0.03 degree Celsius. In the chamber, the scientists maintain the temperature at better than 0.003 degree Celsius.

So, now that Chu and his colleagues built their beamline, have the scientists come? Indeed, the interest in using the HXN has been well above the available time slots. For the three cycles each year, BNL receives about four requests for each available time. This reflects the unique qualities of the instrument, Chu said, adding that he doesn’t expect the rate to drop considerably, even as the HXN continues to operate, because of the ongoing demand.

Researchers have to go through a peer review process, where their ideas are graded for the likelihood of success and for the opportunity to learn from the experiments. All beam time proposals are reviewed by external expert panels, which examine the scientific merit, appropriateness of use of the facility, capability of proposers and quality of prior performance and the research plan and technical feasibility.

Chu fields about 10 calls per month from scientists who want to speak with him about the feasibility of their ideas. He may suggest another station at the NSLS-II or at the Advanced Photon Source at Argonne National Laboratory in Chicago, where he was a beamline scientist starting in 1999.

“I know many of the beamlines” at the Advanced Photon Source, he said. “I recommend some of the potential users to perform experiments at the APS first before coming to the HXN.” By the time scientists arrive at his beamline, Chu said he’s gotten to know them through numerous discussions. He considers them “as a guest” at the HXN hotel. “We try to make sure the experimental needs for the users are met as much as possible,” he said.

The HXN beamline has three staff scientists and two postdoctoral fellows who remain in contact with scientists who use the facility. “For most of the users, at least one of us is working throughout the weekends and late evenings,” said Chu.

Not just a staff scientist, Chu is also a user of the HXN, with currently one active general user proposal through a peer review process in which he is collaborating with Stony Brook University and BNL scientist Esther Takeuchi to explore the nanostructure of metal atoms during phase separation in batteries.

Chu and his wife Youngkyu Park, who works at Cold Spring Harbor Laboratory as a research investigator in basic and preclinical cancer research, live in Northport. The couple’s 22-year-old son Luke is attending Nassau Community College and is planning to transfer to Stony Brook this fall to study engineering. Their daughter Joyce is 18 and is enrolled in the Parsons School of Design in New York.

Chu grew up in Seoul, South Korea, and came to the United States when he was 18. He attended Caltech. While Chu’s parents wanted him to become a doctor, he was more inspired by a cartoon called Astro Boy, in which a scientist, Dr. Tenma, is a hero solving problems. As for the work of the scientists who visit his beamline, Chu said the “success of individual users is the success of the beamline.”

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Chemistry photos for battery press release
A team of researchers led by chemists at the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory has studied an elusive property in cathode materials, called a valence gradient, to understand its effect on battery performance. The findings, published in Nature Communications, demonstrated that the valence gradient can serve as a new approach for stabilizing the structure of high-nickel-content cathodes against degradation and safety issues.

High-nickel-content cathodes have captured the attention of scientists for their high capacity, a chemical property that could power electric vehicles over much longer distances than current batteries support. Unfortunately, the high nickel content also causes these cathode materials to degrade more quickly, creating cracks and stability issues as the battery cycles.

In search of solutions to these structural problems, scientists have synthesized materials made with a nickel concentration gradient, in which the concentration of nickel gradually changes from the surface of the material to its center, or the bulk. These materials have exhibited greatly enhanced stability, but scientists have not been able to determine if the concentration gradient alone was responsible for the improvements. The concentration gradient has traditionally been inseparable from another effect called the valence gradient, or a gradual change in nickel’s oxidation state from the surface of the material to the bulk.

In the new study led by Brookhaven Lab, chemists at DOE’s Argonne National Laboratory synthesized a unique material that isolated the valence gradient from the concentration gradient.

“We used a very unique material that included a nickel valence gradient without a nickel concentration gradient,” said Brookhaven chemist Ruoqian Lin, first author of the study. “The concentration of all three transition metals in the cathode material was the same from the surface to the bulk, but the oxidation state of nickel changed. We obtained these properties by controlling the material’s atmosphere and calcination time during synthesis. With sufficient calcination time, the stronger bond strength between manganese and oxygen promotes the movement of oxygen into the material’s core while maintaining a Ni2+ oxidation state for nickel at the surface, forming the valence gradient.”

Once the chemists successfully synthesized a material with an isolated valence gradient, the Brookhaven researchers then studied its performance using two DOE Office of Science user facilities at Brookhaven Lab—the National Synchrotron Light Source II (NSLS-II) and the Center for Functional Nanomaterials (CFN).

At NSLS-II, an ultrabright x-ray light source, the team leveraged two cutting-edge experimental stations, the Hard X-ray Nanoprobe (HXN) beamline and the Full Field X-ray Imaging (FXI) beamline. By combining the capabilities of both beamlines, the researchers were able to visualize the atomic-scale structure and chemical makeup of their sample in 3-D after the battery operated over multiple cycles.

“Both beamlines have world-leading capabilities. You can’t do this research anywhere else,” said Yong Chu, leader of the imaging and microscopy program at NSLS-II and lead beamline scientist at HXN. “FXI is the fastest nanoscale beamline in the world; it’s about ten times faster than any other competitor. HXN is much slower, but it’s much more sensitive—it’s the highest resolution x-ray imaging beamline in the world.”

HXN beamline scientist Xiaojing Huang added, “At HXN, we routinely run measurements in multimodality mode, which means we collect multiple signals simultaneously. In this study, we used a fluorescence signal and a phytography signal to reconstruct a 3-D model of the sample at the nanoscale. The florescence channel provided the elemental distribution, confirming the sample’s composition and uniformity. The phytography channel provided high-resolution structural information, revealing any microcracks in the sample.”

Meanwhile at FXI, “the beamline showed how the valence gradient existed in this material. And because we conducted full-frame imaging at a very high data acquisition rate, we were able to study many regions and increase the statistical reliability of the study,” Lin said.

At the CFN Electron Microscopy Facility, the researchers used an advanced transmission electron microscope (TEM) to visualize the sample with ultrahigh resolution. Compared to the x-ray studies, the TEM can only probe a much smaller area of the sample and is therefore less statistically reliable across the whole sample, but in turn, the data are far more detailed and visually intuitive.

By combining the data collected across all of the different facilities, the researchers were able to confirm the valence gradient played a critical role in battery performance. The valence gradient “hid” the more capacitive but less stable nickel regions in the center of the material, exposing only the more structurally sound nickel at the surface. This important arrangement suppressed the formation of cracks.

The researchers say this work highlights the positive impact concentration gradient materials can have on battery performance while offering a new, complementary approach to stabilize high-nickel-content cathode materials through the valence gradient.

“These findings give us very important guidance for future novel material synthesis and design of cathode materials, which we will apply in our studies going forward,” Lin said.

This study was a collaborative effort among several universities and DOE laboratories, including research teams involved in DOE’s Battery500 Consortium, which aims to make lithium-metal battery cells with an energy density of 500 watt-hours per kilogram, more than double the energy density of today’s state-of-the-art batteries. The research was supported by DOE’s Office of Energy Efficiency and Renewable Energy, Vehicle Technologies Office and DOE’s Office of Science. Additional x-ray experiments were carried out at the Advanced Light Source (ALS) and the Advanced Photon Source (APS), two DOE Office of Science user facilities that are located at DOE’s Lawrence Berkeley National Laboratory and Argonne National Laboratory, respectively. Operations at NSLS-II, CFN, ALS, and APS are supported by the Office of Science.

Brookhaven National Laboratory is supported by the U.S. Department of Energy’s Office of Science. The Office of Science is the single largest supporter of basic research in the physical sciences in the United States and is working to address some of the most pressing challenges of our time. For more information, visit https://energy.gov/science.

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A rendering of the sauropod known as Mamenchisaurus sinocanadorum, which had a 15-meter-long neck, about 10 feet longer than a typical school bus. Credit: Júlia d'Oliveira

NEWS FROM STONY BROOK UNIVERSITY:

With their long necks and formidable bodies, sauropod dinosaurs have captured people’s imaginations since the first relatively complete sauropod fossils were discovered in the United States in the late 1800s. Now an international team led by Stony Brook University paleontologist Andrew J. Moore, PhD, has revealed that a Late Jurassic Chinese sauropod known as Mamenchisaurus sinocanadorum sported a 15-meter-long neck. The new analysis of this dinosaur, published in the Journal of Systematic Palaeontology, provides fresh insights on the evolution of the iconic sauropod body.

For sauropods, the long neck was the anatomical key to achieving large body size. To power such a large body, sauropods had to be efficient at gathering foodstuffs, and that’s what a long neck was built for. A sauropod could plant itself in one spot and hoover up surrounding vegetation, conserving energy while taking in tons of food. Having a long neck probably also allowed enormous sauropods to shed excess body heat by increasing their surface area, much like the ears of elephants. This way of life – long neck-fueled, quadrupedal gigantism – is not one that is available to mammals or any other form of life today. The sauropod lifestyle was exceptionally successful: their lineage appeared early in dinosaur evolutionary history and persisted until the final days of the Mesozoic, when an asteroid wiped out all dinosaurs (except birds).

Mamenchisaurus sinocanadorum was discovered in approximately 162-million-year-old rocks from the Xinjiang Uyghur Autonomous Region of northwest China in 1987 by the China–Canada Dinosaur Project team, for which it was named in 1993. At approximately 15.1 meters, its neck was more than six times longer than the necks of giraffes, the longest-necked animals alive today, and about 10 feet longer than a typical school bus.

The question of which sauropod had the longest neck is not straightforward. Because of their size, the largest sauropods tend to be some of the most poorly known: it’s very hard to bury such a large animal in sediment and thus safeguard it for fossilization.  Some fragmentary fossils suggest that other sauropod lineages independently evolved necks over 10 meters (32.8 feet) in length. However, poor preservation of these specimens and their closest relatives makes estimates of their neck length speculative.

According to Moore, Assistant Professor in the Department of Anatomical Sciences in the Renaissance School of Medicine at Stony Brook University, although Mamenchisaurus sinocanadorum is known only from a handful of bones from the neck and skull, the research team was able to reconstruct its evolutionary relationships and thus make comparisons to the unusually complete skeletons of its closest relatives. This allowed them to conclude that Mamenchisaurus sinocanadorum had a neck approximately 15.1 meters (49.5 feet) long, the longest neck that can be confidently inferred for any known sauropod.

Their research stems from on-going work to comprehensively document the anatomical diversity and evolutionary history of the family Mamenchisauridae, a radiation of particularly long-necked sauropod dinosaurs that roamed East Asia and possibly other parts of the world from the Middle Jurassic to the Early Cretaceous (approximately ­174–114 million years ago).

“All sauropods were big, but jaw-droppingly long necks didn’t evolve just once,” says Moore. “Mamenchisaurids are important because they pushed the limits on how long a neck can be, and were the first lineage of sauropods to do so. With a 15-meter-long neck, it looks like Mamenchisaurus sinocanadorum might be a record-holder — at least until something longer is discovered.”

How sauropods managed to evolve such long necks and hulking bodies without collapsing under their own weight remains something of a biomechanical puzzle. Remarkable specimens like Mamenchisaurus sinocanadorum provide some clues. For example, like their living cousins, birds, most sauropods had air-filled bones, which would have lightened their skeletons by removing heavy marrow and bone tissue.

Using computed-tomography (CT) scanning, Moore and colleagues found that the vertebrae of Mamenchisaurus sinocanadorum were mostly air (about 69–77% of their volume) – comparable to the lightly built skeletons of storks and other birds.

However, such featherweight skeletons would also be more prone to injury. To combat this, Mamenchisaurus sinocanadorum had 4-meter-long rod-like cervical ribs, bony extensions of the vertebrae that created overlapping bundles of rods on either side of the neck. These bundles would have stiffened the neck of Mamenchisaurus sinocanadorum, increasing its stability and making it possible to build such a lightweight neck.

“Biomechanical studies of the mamenchisaurid neck suggest that it was elevated at only a relatively shallow angle above the horizontal (20-30°). However, even at this relatively shallow angle, the extreme length of the neck would still mean that the animal’s head could reach heights of around 7.5 to 10 m above ground level, facilitating feeding on tree foliage,” says co-author Paul Upchurch, PhD, a Professor of Palaeobiology from the University College London.

“Mamenchisaurus sinocanadorum underscores how much we can learn about sauropod evolution even from very incomplete specimens,” adds co-author Ye Yong, director of the Research Center of Jurassic Stratigraphy and Paleontology at the Zigong Dinosaur Museum in China’s Sichuan Province.

The research was funded by numerous organizations including the United States National Science Foundation, The Royal Society of London, and the National Natural Science Foundation of China.

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District Attorney delivers a special presentation on opioid-related crimes to mayors and other officials from Suffolk County's villages at Lake Grove Village Hall.

Suffolk County Village Officials Association, which represents 32 villages, hosted a special presentation on the opioid crisis Sept. 26 at the Lake Grove Village Hall.

District Attorney Tim Sini (D), Suffolk Police Commissioner Geraldine Hart and Sheriff Errol Toulon Jr. (D) all spoke to the group about how the crisis has fueled a regional surge in illegal firearms seizures and sex trafficking crimes.

Most criminal cases in the county, the officials said, relate to opioid epidemic.

People initially became addicted to prescription painkillers and over time, as demand increased, supply went down, and prices went up. So, people gravitated toward heroin, the DA said, which is more potent and more dangerous. Drug dealers, who realized that money can be made, began cutting their product with the synthetic opioid fentanyl, and more recently with fentanyl variations known as analogs. Fentanyl, Sini said, originates in China and is coming into the United States through the Mexican border. The drug is also being sent into the U.S. over the Canadian border and from China through the U.S. mail.

County officials said they are drilling down as hard as possible. 

Since 2016, the federal government assigned an analyst exclusively to Suffolk County Police Department to examine overdose information with maps and weekly and monthly overdose reports. The mapping system, known as High Intensity Drug Trafficking Areas program, or HIDTA, provides a real-time picture of overdoses. It also helps identify and coordinate candidates for the county’s preventing incarceration via opportunities for treatment program known as PIVOT for short. 

“Everything we do is driven by analytics,” Hart said.

The county has also been using court-sanctioned surveillance methods such as phone tapping and search warrants to crack down on drug crimes. It issued more than 350 narcotics search warrants in 2018 and has eavesdropped on more than 150 phone lines. Consequently, the county has seized greater amounts of certain drugs and illegal firearms. 

The officials said during their presentation that it’s targeting dealers who cause overdoses and charging them with manslaughter. Sini said that through surveillance, he’s learning that tougher manslaughter statutes result in dealers turning away from deadly drugs to instead
peddle nonlethal drugs. 

In 2018, the county also launched a sex trafficking unit that has identified and interviewed more than 200 sex trafficking victims. It has arrested 34 people for 235 counts of sex-trafficking related charges and learned during the interviews how drug traffickers use opioids to addict young women to keep them dependent.

Toulon said that they’re gathering information while the women are in the sheriff’s facility, which is providing other useful information on drug and sex traffickers. 

Victims, while in the sheriff’s facility, are involved in vocational and educational programs and put in touch with nongovernmental organizations that assist with counseling, drug treatment and job training.  A big problem, though, Toulon said, is housing.  

County officials emphasized that human trafficking is happening right here, right now in our communities. It can affect anyone from your neighbor to your niece and nephew. 

Officials are also calling for the use of different terminology for prostitution.  

“It’s a modern-day form of slavery and needs to be called what it is: sex trafficking,” Hart said. The force has historically arrested the women and that was the case, Hart said, but the county’s approach is shifting and officials are now looking at the women as victims.  

Officials are asking people to trust their own  instincts. 

“If you’re at a 7-Eleven and you see an older man in a car with a young woman who looks distressed, call or text us,” the officials said.

The county initiated a Text-a-Tip program. To reach officials, text TIP SUFFOLK to the number 888-777. Residents can confidentially share any information related to illicit or suspicious activity, including drug use or trafficking, Toulon said. 

Paul Tonna, who serves as executive director of the village organization, said in a telephone interview after the event that a group of mayors were previously given a private presentation on the topic in graphic detail. The situation, he said, is horrible. The women are being forced to perform six or seven sex acts a day. He is calling for people such as PTAs and religious groups to sponsor awareness campaigns with officials.

Local villages have resources, Tonna said, such as constabulary that can also become the eyes and ears of county officials. 

“We’re not here to say you need to do more,” Sini said. ”We need to think outside of the box. Because of collective efforts, we can make greater strides.”

Ann Marie Csorny is director of Suffolk County Department of Health Services’ Community Mental Hygiene Services.  The Prevention Resource Center, run by the Family Service League, she said, offers effective tools for those working to prevent drug and alcohol abuse.  Villages and towns, she said, should tap into coalitions that exist or start to build their own coalitions.

“Communities can have a great impact in terms of preventing or reducing drug use, alcohol abuse and related problems when they understand and promote coalition building,” she said. “This can be very exciting in that involved communities promote civic engagement and the building of shared understanding, shared norms, shared values, trust, and cooperation.”

 

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From left, BNL Staff Scientist Lihua Zhang, former postdoctoral researcher Vitor Manfrinato and BNL Senior Scientist Aaron Stein. Photo courtesy of BNL

By Daniel Dunaief

It took a village to build this particular village or, more precisely, a pattern so small it could fit thousands of times over on the head of a pin.

Working at Brookhaven National Laboratory’s Center for Functional Nanomaterials, a team of researchers wanted to exceed the boundaries of creating small patterns with finely honed features. The group included Aaron Stein, a senior scientist at CFN, Charles Black, the head of CFN, Vitor Manfrinato, a former postdoctoral researcher at BNL and several other key members of the BNL team. The team added a pattern generator that allowed them to control a microscope to create a pattern that set a record for drawing at the 1-nanometer scale.

Just for reference, the width of a human hair is about 80,000 to 100,000 nanometers. The size of the pattern is a breakthrough as standard tools and processes generally produce patterns on a scale of 10 nanometers. “We were able to push that by a factor of five or 10 below,” Stein said. “When you get to those small size scales, that’s pretty significant.”

In this case, the novelty that enabled this resolution originated with the idea of employing the scanning transmission electron microscope, which isn’t typically used for patterning to create these images. The scanning transmission electron microscope has an extraordinarily high resolution, while the pattern generator allowed them to control the patterns they drew and other aspects of the exposure.

Researchers at CFN are focusing on this spectacularly small world to manipulate properties such as chemical reactivity, electrical conductivity and light interactions. “This new development is exciting because it will allow other researchers to create nanomaterials at previously impossible size scales,” Kevin Yager, a group leader at CFN explained in an email. “There are numerous predictions about how materials should behave differently at a size scale at 1 to 3 nanometers. With this patterning capability, we can finally test some of those hypotheses,” he said.

Stein and the research team were able to create this pattern on a simple polymer, polymethyl methacrylate, or PMMA for short. “It’s surprising to us that you don’t need fancy materials to create these kinds of features,” said Stein. “PMMA is a common polymer. It’s Plexiglas. It’s kind of exciting to do something that is beyond what people have done” up until now.

One of the many possible next steps, now that the researchers have developed this proof of principle, is to apply this technique to a substance that might have commercial use. Taking the same approach with silicon, for example, could lead to innovations in electronics. “We can make them with a high clarity of patterns and sharp corners, which we can’t do with other techniques,” Stein said.

The BNL research team would “like to apply this to real world research,” which could include electronics and transistors, as well as photonics and plasmonics, he added. This project arose out of a doctoral thesis that Manfrinato was conducting. He is one of the many scientists who came to BNL, which isa Department of Energy funded user facility that provides tools to conduct research for scientists from around the world.

Manfrinato was a doctoral student in Professor Karl Berggren’s group at the Massachusetts Institute of Technology. In an email, Manfrinato explained that he was interested in pushing the resolution limits of e-beam lithography. “BNL has state of the art facilities and expert staff, so our collaboration was a great fit, starting in 2011,” he explained.

Other scientists thought it was worthwhile to continue to pursue this effort, encouraging him to “come here and work on this. It’s a home grown project,” Stein said. Manfrinato worked on his doctorate from 2011 to 2015, at which point he became a postdoctoral researcher at BNL. His efforts involved several groups, all within the Center for Functional Nanomaterials at BNL. Stein, Manfrinato and Black worked on the lithography part of the project, while Lihua Zhang and Eric Stach developed the microscopy. Yager helped the team to understand the processes by which they could pattern PMMA at such small scale lengths.

“No one or two of us could have made this happen,” Stein said. “That’s really the joy of working in a place like this: There are [so many] permutations for collaborating.” Indeed, the other scientists involved in this study were Yager; Zhang, a staff scientist in electron microscopy; Stach, the electron microscopy group leader at CFN; and Chang-Yong Nam, who assisted with the pattern transfer.

Manfrinato, who is now a research and development engineer at a startup company in the San Francisco Bay area, explained that this lithographic technique has numerous possible applications. Other researchers could create prototypes of their devices at a level below the 10-nanometer scale at CFN. Manfrinato interacts with the BNL team a few times a month and he has “exciting results to be further analyzed, explored and published,” he wrote in an email.

Stein said BNL would like to offer this patterning device for other users who come to BNL. Ultimately, researchers use materials at this scale to find properties that may vary when the materials are larger. Sometimes, the properties such as color, chemical reactivity, electrical conductivity and light interactions change enough to create opportunities for new products, innovations or more efficient designs.

A resident of Huntington, Stein and his wife Sasha Abraham, who works in the planning department for the Town of Huntington, have a 15-year-old daughter Lily and a 13-year-old son Henry.

As for his work, Stein said he’s interested in continuing to push the limits of understanding various properties of nanomaterials. “My career has been using the e-beam lithography to make all sorts of structures,” he said. “We’re in a regime where people have not been there before. Finding the bottom is very interesting. Figuring out the limits of this technique is, in and of itself” an incredible opportunity.

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