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  • richardmitnick 11:15 am on March 31, 2017 Permalink | Reply
    Tags: , Catalysis, Methanol, , NSLS-II   

    From BNL: “Chemists ID Catalytic ‘Key’ for Converting CO2 to Methanol” 

    Brookhaven Lab

    March 23, 2017
    Karen McNulty Walsh,
    (631) 344-8350
    kmcnulty@bnl.gov

    Peter Genzer
    (631) 344-3174
    genzer@bnl.gov

    Results will guide design of improved catalysts for transforming pollutant to useful chemicals.

    1
    Jingguang Chen and Jose Rodriguez (standing) discuss the catalytic mechanism with Ping Liu and Shyam Kattel (seated).

    Capturing carbon dioxide (CO2) and converting it to useful chemicals such as methanol could reduce both pollution and our dependence on petroleum products. So scientists are intensely interested in the catalysts that facilitate such chemical conversions. Like molecular dealmakers, catalysts bring the reacting chemicals together in a way that makes it easier for them to break and rearrange their chemical bonds. Understanding details of these molecular interactions could point to strategies to improve the catalysts for more energy-efficient reactions.

    With that goal in mind, chemists from the U.S. Department of Energy’s Brookhaven National Laboratory and their collaborators just released results from experiments and computational modeling studies that definitively identify the “active site” of a catalyst commonly used for making methanol from CO2. The results, published in the journal Science, resolve a longstanding debate about exactly which catalytic components take part in the chemical reactions—and should be the focus of efforts to boost performance.

    “This catalyst—made of copper, zinc oxide, and aluminum oxide—is used in industry, but it’s not very efficient or selective,” said Brookhaven chemist Ping Liu, the study’s lead author, who also holds an adjunct position at nearby Stony Brook University (SBU). “We want to improve it, and get it to operate at lower temperatures and lower pressures, which would save energy,” she said.

    But prior to this study, different groups of scientists had proposed two different active sites for the catalyst—a portion of the system with just copper and zinc atoms, or a portion with copper zinc oxide.

    “We wanted to know which part of the molecular structure binds and breaks and makes bonds to convert reactants to product—and how it does that,” said co-author Jose Rodriguez, another Brookhaven chemist associated with SBU.

    To find out, Rodriguez performed a series of laboratory experiments using well-defined model catalysts, including one made of zinc nanoparticles supported on a copper surface, and another with zinc oxide nanoparticles on copper. To tell the two apart, he used an energetic x-ray beam to zap the samples, and measured the properties of electrons emitted. These electronic “signatures” contain information about the oxidation state of the atoms the electrons came from—whether zinc or zinc oxide.

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    Brookhaven chemist Ping Liu

    Meanwhile Liu, Jingguang Chen of Brookhaven Lab and Columbia University, and Shyam Kattel, the first author of the paper and a postdoctoral fellow co-advised by Liu and Chen, used computational resources at Brookhaven’s Center for Functional Nanomaterials (CFN) and the National Energy Research Scientific Computing Center (NERSC)—two DOE Office of Science User Facilities—to model how these two types of catalysts would engage in the CO2-to-methanol transformations. These theoretical studies use calculations that take into account the basic principles of breaking and making chemical bonds, including the energy required, the electronic states of the atoms, and the reaction conditions, allowing scientists to derive the reaction rates and determine which catalyst will give the best rate of conversion.

    “We found that copper zinc oxide should give the best results, and that copper zinc is not even stable under reaction conditions,” said Liu. “In fact, it reacts with oxygen and transforms to copper zinc oxide.”

    Those predictions matched what Rodriguez observed in the laboratory. “We found that all the sites participating in these reactions were copper zinc oxide,” he said.

    But don’t forget the copper.

    “In our simulations, all the reaction intermediates—the chemicals that form on the pathway from CO2 to methanol—bind at both the copper and zinc oxide,” Kattel said. “So there’s a synergy between the copper and zinc oxide that accelerates the chemical transformation. You need both the copper and the zinc oxide.”

    3
    Ping Liu and Shyam Kattel with the x-ray source used in this study.

    Optimizing the copper/zinc oxide interface will become the driving principal for designing a new catalyst, the scientists say.

    “This work clearly demonstrates the synergy from combining theoretical and experimental efforts for studying catalytic systems of industrial importance,” said Chen. “We will continue to utilize the same combined approaches in future studies.”

    For example, said Rodriguez, “We’ll try different configurations of the atoms at the copper/zinc oxide interface to see how that affects the reaction rate. Also, we’ll be going from studying the model system to systems that would be more practical for use by industry.”

    An essential tool for this next step will be Brookhaven’s National Synchrotron Light Source II (NSLS-II), another Office of Science User Facility. NSLS-II produces extremely bright beams of x-rays—about 10,000 times brighter than the broad-beam laboratory x-ray source used in this study. Those intense x-ray beams will allow the scientists to take high-resolution snapshots that reveal both structural and chemical information about the catalyst, the reactants, and the chemical intermediates that form as the reaction occurs.

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    Brookhaven scientists identified how a zinc/copper (Zn/Cu) catalyst transforms carbon dioxide (two red and one grey balls) and hydrogen (two white balls) to methanol (one grey, one red, and four white balls), a potential fuel. Under reaction conditions, Zn/Cu transforms to ZnO/Cu, where the interface between the ZnO and Cu provides the active sites that allow the formation of methanol.

    “And we’ll continue to expand the theory,” said Liu. “The theory points to the mechanistic details. We want to modify interactions at the copper/zinc oxide interface to see how that affects the activity and efficiency of the catalyst, and we’ll need the theory to move forward with that as well.”

    An additional co-author, Pedro Ramírez of Universidad Central de Venezuela, made important contributions to this study by helping to test the activity of the copper zinc and copper zinc oxide catalysts.

    This research was supported by the DOE Office of Science.

    See the full article here .

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    One of ten national laboratories overseen and primarily funded by the Office of Science of the U.S. Department of Energy (DOE), Brookhaven National Laboratory conducts research in the physical, biomedical, and environmental sciences, as well as in energy technologies and national security. Brookhaven Lab also builds and operates major scientific facilities available to university, industry and government researchers. The Laboratory’s almost 3,000 scientists, engineers, and support staff are joined each year by more than 5,000 visiting researchers from around the world. Brookhaven is operated and managed for DOE’s Office of Science by Brookhaven Science Associates, a limited-liability company founded by Stony Brook University, the largest academic user of Laboratory facilities, and Battelle, a nonprofit, applied science and technology organization.
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  • richardmitnick 9:02 am on February 23, 2017 Permalink | Reply
    Tags: , Catalysis, , Light-driven reaction converts carbon dioxide into fuel, , , Rhodium nanoparticles   

    From Duke via phys.org: “Light-driven reaction converts carbon dioxide into fuel” 

    Duke Bloc
    Duke Crest

    Duke University

    phys.org

    phys.org

    February 23, 2017

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    Duke University researchers have engineered rhodium nanoparticles (blue) that can harness the energy in ultraviolet light and use it to catalyze the conversion of carbon dioxide to methane, a key building block for many types of fuels. Credit: Chad Scales

    Duke University researchers have developed tiny nanoparticles that help convert carbon dioxide into methane using only ultraviolet light as an energy source.

    Having found a catalyst that can do this important chemistry using ultraviolet light, the team now hopes to develop a version that would run on natural sunlight, a potential boon to alternative energy.

    Chemists have long sought an efficient, light-driven catalyst to power this reaction, which could help reduce the growing levels of carbon dioxide in our atmosphere by converting it into methane, a key building block for many types of fuels.

    Not only are the rhodium nanoparticles made more efficient when illuminated by light, they have the advantage of strongly favoring the formation of methane rather than an equal mix of methane and undesirable side-products like carbon monoxide. This strong “selectivity” of the light-driven catalysis may also extend to other important chemical reactions, the researchers say.

    “The fact that you can use light to influence a specific reaction pathway is very exciting,” said Jie Liu, the George B. Geller professor of chemistry at Duke University. “This discovery will really advance the understanding of catalysis.”

    The paper appears online Feb. 23 in Nature Communications.

    Despite being one of the rarest elements on Earth, rhodium plays a surprisingly important role in our everyday lives. Small amounts of the silvery grey metal are used to speed up or “catalyze” a number of key industrial processes, including those that make drugs, detergents and nitrogen fertilizer, and they even play a major role breaking down toxic pollutants in the catalytic converters of our cars.

    Rhodium accelerates these reactions with an added boost of energy, which usually comes in the form of heat because it is easily produced and absorbed. However, high temperatures also cause problems, like shortened catalyst lifetimes and the unwanted synthesis of undesired products.

    2
    Rhodium nanocubes were observed under a transmission electron microscope. Credit: Xiao Zhang

    In the past two decades, scientists have explored new and useful ways that light can be used to add energy to bits of metal shrunk down to the nanoscale, a field called plasmonics.

    “Effectively, plasmonic metal nanoparticles act like little antennas that absorb visible or ultraviolet light very efficiently and can do a number of things like generate strong electric fields,” said Henry Everitt, an adjunct professor of physics at Duke and senior research scientist at the Army’s Aviation and Missile RD&E Center at Redstone Arsenal, AL. “For the last few years there has been a recognition that this property might be applied to catalysis.”

    Xiao Zhang, a graduate student in Jie Liu’s lab, synthesized rhodium nanocubes that were the optimal size for absorbing near-ultraviolet light. He then placed small amounts of the charcoal-colored nanoparticles into a reaction chamber and passed mixtures of carbon dioxide and hydrogen through the powdery material.

    When Zhang heated the nanoparticles to 300 degrees Celsius, the reaction generated an equal mix of methane and carbon monoxide, a poisonous gas. When he turned off the heat and instead illuminated them with a high-powered ultraviolet LED lamp, Zhang was not only surprised to find that carbon dioxide and hydrogen reacted at room temperature, but that the reaction almost exclusively produced methane.

    “We discovered that when we shine light on rhodium nanostructures, we can force the chemical reaction to go in one direction more than another,” Everitt said. “So we get to choose how the reaction goes with light in a way that we can’t do with heat.”

    This selectivity—the ability to control the chemical reaction so that it generates the desired product with little or no side-products—is an important factor in determining the cost and feasibility of industrial-scale reactions, Zhang says.

    “If the reaction has only 50 percent selectivity, then the cost will be double what it would be if the selectively is nearly 100 percent,” Zhang said. “And if the selectivity is very high, you can also save time and energy by not having to purify the product.”

    Now the team plans to test whether their light-powered technique might drive other reactions that are currently catalyzed with heated rhodium metal. By tweaking the size of the rhodium nanoparticles, they also hope to develop a version of the catalyst that is powered by sunlight, creating a solar-powered reaction that could be integrated into renewable energy systems.

    “Our discovery of the unique way light can efficiently, selectively influence catalysis came as a result of an on-going collaboration between experimentalists and theorists,” Liu said. “Professor Weitao Yang’s group in the Duke chemistry department provided critical theoretical insights that helped us understand what was happening. This sort of analysis can be applied to many important chemical reactions, and we have only just begun to explore this exciting new approach to catalysis.”

    Read more at: https://phys.org/news/2017-02-light-driven-reaction-carbon-dioxide-fuel.html#jCp

    See the full article here .

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    Younger than most other prestigious U.S. research universities, Duke University consistently ranks among the very best. Duke’s graduate and professional schools — in business, divinity, engineering, the environment, law, medicine, nursing and public policy — are among the leaders in their fields. Duke’s home campus is situated on nearly 9,000 acres in Durham, N.C, a city of more than 200,000 people. Duke also is active internationally through the Duke-NUS Graduate Medical School in Singapore, Duke Kunshan University in China and numerous research and education programs across the globe. More than 75 percent of Duke students pursue service-learning opportunities in Durham and around the world through DukeEngage and other programs that advance the university’s mission of “knowledge in service to society.”

     
  • richardmitnick 7:34 am on July 29, 2015 Permalink | Reply
    Tags: , Catalysis, ,   

    From Princeton: “New chemistry makes strong bonds weak” 

    Princeton University
    Princeton University

    July 28 2015
    Tien Nguyen

    Researchers at Princeton have developed a new chemical reaction that breaks the strongest bond in a molecule instead of the weakest, completely reversing the norm for reactions in which bonds are evenly split to form reactive intermediates.

    1
    Catalytic alkene carboamination enabled by oxidative proton-coupled electron transfer

    Published on July 13 in the Journal of the American Chemical Society, the non-conventional reaction is a proof of concept that will allow chemists to access compounds that are normally off-limits to this pathway. The team used a two-component catalyst system that works in tandem to selectively activate the strongest bond in the molecule, a nitrogen-hydrogen (N-H) bond, through a process known as proton-coupled electron transfer (PCET).

    “This PCET chemistry was really interesting to us. In particular, the idea that you can use catalysts to modulate an intrinsic property of a molecule allows you to access chemical space that you couldn’t otherwise,” said Robert Knowles, an assistant professor of chemistry who led the research.

    Using PCET as a way to break strong bonds is seen in many essential biological systems, including photosynthesis and respiration, he said. Though this phenomenon is known in biological and inorganic chemistry settings, it hasn’t been widely applied to making new molecules—something Knowles hopes to change.

    Given the unexplored state of PCET catalysis, Knowles decided to turn to theory instead of the trial and error approach usually taken by synthetic chemists in the initial stages of reaction development. Using a simple mathematical formula, the researchers calculated, for any pair of catalysts, the pair’s combined “effective bond strength,” which is the strength of the strongest bond they could break. Because both molecules independently contribute to this value, the research team had a high degree of flexibility in designing the catalyst system.

    When they tested the catalyst pairs in the lab, the researchers observed a striking correlation between the “effective bond strength” and the reaction efficiency. While effective bond strengths that were lower or higher than the target N-H bond strength gave low reaction yields, the researchers found that matching the strengths promoted the reaction in very high yield.

    “To see this formula actually working was really inspiring,” said Gilbert Choi, a graduate student in the Knowles lab and lead author on the work. Once he identified a successful catalyst system, he explored the scope of the reaction and its mechanism.

    2
    Proposed catalytic cycle

    The researchers think that the reaction starts with one of the catalysts, a compound called dibutylphosphate, tugging on a hydrogen atom, which lengthens and weakens the N-H bond. At the same time, the other catalyst, known as a light-activated iridium complex, targets the weakened bond and plucks off one electron from the two-electron bond, slicing it down the middle.

    Once the bond is split, the reactive nitrogen intermediate goes on to form a new carbon-nitrogen bond, giving rise to structurally complex products. This finding builds on work the Knowles lab published earlier this year also in the Journal of the American Chemical Society on a similar reaction that used a more sensitive catalyst system.

    Their research has laid a solid foundation for PCET catalysis as a platform for developing new reactions. “My sincere view is that ideas are a lot more valuable than reactions,” Knowles said. “I’m optimistic that people can use these ideas and do things that we hadn’t even considered.”

    See the full article here.

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    As a world-renowned research university, Princeton seeks to achieve the highest levels of distinction in the discovery and transmission of knowledge and understanding. At the same time, Princeton is distinctive among research universities in its commitment to undergraduate teaching.

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  • richardmitnick 5:32 pm on February 13, 2015 Permalink | Reply
    Tags: , Catalysis, , , , ,   

    From SLAC: “Scientists Get First Glimpse of a Chemical Bond Being Born” 


    SLAC Lab

    February 12, 2015

    Scientists have used an X-ray laser at the Department of Energy’s SLAC National Accelerator Laboratory to get the first glimpse of the transition state where two atoms begin to form a weak bond on the way to becoming a molecule.

    1
    This illustration shows atoms forming a tentative bond, a moment captured for the first time in experiments with an X-ray laser at SLAC National Accelerator Laboratory. The reactants are a carbon monoxide molecule, left, made of a carbon atom (black) and an oxygen atom (red), and a single atom of oxygen, just to the right of it. They are attached to the surface of a ruthenium catalyst, which holds them close to each other so they can react more easily. When hit with an optical laser pulse, the reactants vibrate and bump into each other, and the carbon atom forms a transitional bond with the lone oxygen, center. The resulting carbon dioxide molecule detaches and floats away, upper right. The Linac Coherent Light Source (LCLS) X-ray laser probed the reaction as it proceeded and allowed the movie to be created. (SLAC National Accelerator Laboratory)

    This fundamental advance, reported Feb. 12 in Science Express and long thought impossible, will have a profound impact on the understanding of how chemical reactions take place and on efforts to design reactions that generate energy, create new products and fertilize crops more efficiently.

    “This is the very core of all chemistry. It’s what we consider a Holy Grail, because it controls chemical reactivity,” said Anders Nilsson, a professor at the SLAC/Stanford SUNCAT Center for Interface Science and Catalysis and at Stockholm University who led the research. “But because so few molecules inhabit this transition state at any given moment, no one thought we’d ever be able to see it.”


    Anders Nilsson, a professor at SLAC and at Stockholm University, explains how scientists used an X-ray laser to watch atoms form a tentative bond, and why that’s important.

    The experiments took place at SLAC’s Linac Coherent Light Source (LCLS), a DOE Office of Science User Facility. Its brilliant, strobe-like X-ray laser pulses are short enough to illuminate atoms and molecules and fast enough to watch chemical reactions unfold in a way never possible before.

    Researchers used LCLS to study the same reaction that neutralizes carbon monoxide (CO) from car exhaust in a catalytic converter. The reaction takes place on the surface of a catalyst, which grabs CO and oxygen atoms and holds them next to each other so they pair up more easily to form carbon dioxide.

    In the SLAC experiments, researchers attached CO and oxygen atoms to the surface of a ruthenium catalyst and got reactions going with a pulse from an optical laser. The pulse heated the catalyst to 2,000 kelvins – more than 3,000 degrees Fahrenheit – and set the attached chemicals vibrating, greatly increasing the chance that they would knock into each other and connect.

    The team was able to observe this process with X-ray laser pulses from LCLS, which detected changes in the arrangement of the atoms’ electrons – subtle signs of bond formation – that occurred in mere femtoseconds, or quadrillionths of a second.

    “First the oxygen atoms get activated, and a little later the carbon monoxide gets activated,” Nilsson said. “They start to vibrate, move around a little bit. Then, after about a trillionth of a second, they start to collide and form these transition states.”

    ‘Rolling Marbles Uphill’

    The researchers were surprised to see so many of the reactants enter the transition state – and equally surprised to discover that only a small fraction of them go on to form stable carbon dioxide. The rest break apart again.

    “It’s as if you are rolling marbles up a hill, and most of the marbles that make it to the top roll back down again,” Nilsson said. “What we are seeing is that many attempts are made, but very few reactions continue to the final product. We have a lot to do to understand in detail what we have seen here.”

    Theory played a key role in the experiments, allowing the team to predict what would happen and get a good idea of what to look for. “This is a super-interesting avenue for theoretical chemists. It’s going to open up a completely new field,” said report co-author Frank Abild-Pedersen of SLAC and SUNCAT.

    A team led by Associate Professor Henrik Öström at Stockholm University did initial studies of how to trigger the reactions with the optical laser. Theoretical spectra were computed under the leadership of Stockholm Professor Lars G.M. Pettersson, a longtime collaborator with Nilsson.

    Preliminary experiments at SLAC’s Stanford Synchrotron Radiation Lightsource (SSRL), another DOE Office of Science User Facility, also proved crucial. Led by SSRL’s Hirohito Ogasawara and SUNCAT’s Jerry LaRue, they measured the characteristics of the chemical reactants with an intense X-ray beam so researchers would be sure to identify everything correctly at the LCLS, where beam time is much more scarce. “Without SSRL this would not have worked,” Nilsson said.

    The team is already starting to measure transition states in other catalytic reactions that generate chemicals important to industry.

    “This is extremely important, as it provides insight into the scientific basis for rules that allow us to design new catalysts,” said SUNCAT Director and co-author Jens Nørskov.

    Researchers from LCLS, Helmholtz-Zentrum Berlin for Materials and Energy, University of Hamburg, Center for Free Electron Laser Science, University of Potsdam, Fritz-Haber Institute of the Max Planck Society, DESY and University of Liverpool also contributed to the research. The research was funded by the DOE Office of Science, the Swedish National Research Council, the Knut and Alice Wallenberg Foundation, the Volkswagen Foundation and the German Research Foundation (DFG) Center for Ultrafast Imaging.

    See the full article here.

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    SLAC is a multi-program laboratory exploring frontier questions in photon science, astrophysics, particle physics and accelerator research. Located in Menlo Park, California, SLAC is operated by Stanford University for the DOE’s Office of Science.
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  • richardmitnick 5:14 pm on April 10, 2013 Permalink | Reply
    Tags: , Catalysis, ,   

    From Berkeley Lab: “…Black Nanoparticles Could Play Key Role in Clean Energy Photocatalysis” 


    Berkeley Lab

    “A unique atomic-scale engineering technique for turning low-efficiency photocatalytic “white” nanoparticles of titanium dioxide into high-efficiency “black” nanoparticles could be the key to clean energy technologies based on hydrogen.

    Samuel Mao, a scientist who holds joint appointments with Berkeley Lab’s Environmental Energy Technologies Division and the University of California at Berkeley, leads the development of a technique for engineering disorder into the nanocrystalline structure of the semiconductor titanium dioxide. This turns the naturally white crystals black in color, a sign that the crystals are now able to absorb infrared as well as visible and ultraviolet light. The expanded absorption spectrum substantially improves the efficiency with which black titanium dioxide can use sunlight to split water molecules for the production of hydrogen.

    swm
    Berkeley Lab’s Samuel Mao used disorder engineering to transform titanium nanocrystals into highly efficient solar hydrogen photocatalysts, a transformation marked by turning the crystals from white to black. (Photo by Roy Kaltschmidt)

    ‘We have demonstrated that black titanium dioxide nanoparticles are capable of generating hydrogen through solar-driven photocatalytic reactions with a record-high efficiency,’ Mao said in a talk at the American Chemical Society (ACS)’s national meeting in New Orleans.

    ‘The synthesis of black titanium dioxide nanoparticles was based on a hydrogenation process in which white titanium dioxide nanocrystals were subjected to high pressure hydrogen gas,’ said Mao. ‘The unique disordered structure creates a photocatalyst that is both durable and efficient, and gives titanium dioxide, one of the most-studied of all oxide materials, a renewed potential.’”

    See the full article here.

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  • richardmitnick 2:08 pm on March 18, 2012 Permalink | Reply
    Tags: , Catalysis, ,   

    From Brookhaven Lab: “New Catalyst for Safe, Reversible Hydrogen Storage” 

    Room-temperature reaction takes place in water; can switch from hydrogen storage to release by changing pH

    Karen McNulty Walsh
    March 18, 2012

    “Scientists at the U.S. Department of Energy’s (DOE) Brookhaven National Laboratory and collaborators have developed a new catalyst that reversibly converts hydrogen gas and carbon dioxide to a liquid under very mild conditions. The work — described in a paper published online March 18, 2012, in Nature Chemistry — could lead to efficient ways to safely store and transport hydrogen for use as an alternative fuel.

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    This diagram shows the new catalyst in its protonated and deprotonated states as it reversibly converts hydrogen and CO2 gas to and from liquid formate or formic acid at ambient temperature and pressure. The gases can thereby be stored and transported as a liquid, and used later in carbon-neutral energy applications, simply by adjusting the pH. NO image credit.

    Interested? See the full article here.

    One of ten national laboratories overseen and primarily funded by the Office of Science of the U.S. Department of Energy (DOE), Brookhaven National Laboratory conducts research in the physical, biomedical, and environmental sciences, as well as in energy technologies and national security. Brookhaven Lab also builds and operates major scientific facilities available to university, industry and government researchers. Brookhaven is operated and managed for DOE’s Office of Science by Brookhaven Science Associates, a limited-liability company founded by Stony Brook University, the largest academic user of Laboratory facilities, and Battelle, a nonprofit, applied science and technology organization.
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