Argonne National Laboratory Center for Nanoscale Materials U.S. Department of Energy

Amanda Petford-LongThe CNM has had a busy few months since our last newsletter, despite the holiday break and our planned maintenance period in January. The latter are continuing to prove very valuable, allowing us to minimize the disruptions to users and staff that can occur when maintenance activities occur on a more ad hoc basis. We have had some questions from users regarding the frequency of the planned maintenance periods — let me assure you that we make full use of the time available: a considerable number of activities are carried out during each period, with several of these being preventative maintenance that will hopefully reduce unplanned downtime at other points during the year.

An organizational change at Argonne has been the creation of the Nanoscience and Technology Division, which now houses both the Center for Nanoscale Materials and the Electron Microscopy Center. These changes were made to better align the Laboratory's nanoscience program with the established organizational structure at Argonne, but CNM users should not expect to see any changes to operation of the CNM facility or user program.

I am also delighted to announce the new membership of the Scientific Advisory Committee (SAC) for CNM, which now includes three members from industrial organizations, in addition to six from academic institutions and one from a national laboratory. I am very grateful indeed for the dedication that our SAC and our User Executive Committee (UEC) show to promoting excellence within the CNM, and I would encourage any of our users with questions or comments about CNM to contact members of the SAC or UEC, in addition to the CNM staff.

We are fortunate as always with the very high quality of staff and postdoctoral researchers that we attract to CNM. In October 2012, Guoren Bai joined us from the Materials Science Division at Argonne to provide user support in the clean room, and other staff updates can be found further in this newsletter. A new venture for CNM has been to provide lecturers for a graduate lecture series on nanomaterials at Northwestern University. Staff members have given well-received lectures on their specialist areas, and I am grateful for the time they have committed to this outreach activity.

I wish you all a belated Happy New Year and I hope that we will continue to provide the high-quality user experience that you have come to expect during your visits to CNM.

Amanda Petford-Long, CNM Director

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Call for Proposals Deadline: March 8, 2013

The system is now open for submissions. We look forward to the possibility of hosting your exciting and innovative nanoscience and nanotechnology projects. (More >>)

APS/CNM/EMC Users Meeting: May 6-9, 2013

Registration is now open for the next Argonne APS/CNM/EMC Users Meeting, themed "Building on Success: Focus on the Future," takes place on May 6-9, 2013. Cross-facility workshops on imaging, batteries, and analysis, and visualization & data management will highlight, promote, and stimulate user science from the CNM, the Advanced Photon Source, and Electron Microscopy Center. In addition, there will be keynote and plenary science lectures, a CNM workshop on carbons for NEMS and nanoelectronics, facility status updates, poster sessions, a vendor expo, short courses, and social events. Users are invited to contribute poster presentations of their results, and there will be a best student poster competition. Complete meeting details are available online.

Workshop on User Facilities for Industry 101

The APS, CNM, and EMC user facilities invite industrial scientists and engineers to attend a one-day workshop on May 9, 2013, to learn more about Argonne National Laboratory and its capabilities and techniques that are available for use by industry. This workshop will showcase several successful industrial user experiments, as well as explain the different ways in which industrial scientists can work with Argonne scientists. Representatives from these user facilities as well as from Argonne's Technology Development and Commercialization Division will be available to conduct one-on-one discussions regarding the feasibility of research ideas, proprietary research opportunities, etc. The workshop will conclude with facility tours and give participants the opportunity to interact directly with scientists. This event is being held as a satellite workshop of the APS/CNM/EMC Users Meeting, which participants can choose to register for as well.

nanoMATTERS is Born: New Newsletter Name

Alert readers may have noticed a difference in the masthead for this February 2013 issue. After the October 2012 of the CNM Newsletter, the CNM held a division-wide contest to find a new name: nanoMATTERS!

CNM Maintenance Shutdown Period: May 13-19, 2013

To better ensure reliable instrument availability at CNM, defined maintenance periods occur three times per calendar year. During these times, the CNM is not available for onsite user activities. The maintenance periods, lasting a maximum of one week each, are used to perform preventive maintenance on the scientific instruments and their support equipment. In addition, the facility's operating infrastructure systems will undergo preventive maintenance that will help avoid unplanned shutdowns. The next maintenance period occurs May 13-19, 2013.

Onsite Winter Shuttle Transportation Now Available

The GreenLab Shuttle is running at the Argonne site until March 29, 2013. It encourages green commuting by providing transportation from the main gate and across campus. The shuttle runs during the cold season; Bike Share bikes are available to employees and users (a training course is required) during warm weather months. The GreenLab Shuttle has a predefined route and schedule that includes the CNM and the Argonne Guest House. Main Gate morning pickup times are 7:35, 8:15, and 8:55 a.m. The shuttle also will drop passengers off at the Main Gate at 4:45 and 5:20 p.m., convenient for Pace bus route 715. A schedule and map are available online.

2013 NUFO Exhibit on Capitol Hill

The National User Facility Organization (NUFO) represents the interests of users who conduct research at U.S. national scientific user facilities. NUFO has been invited by the House Science & National Labs Caucus to help demonstrate to Congressional representatives how scientists who use our nation's user facilities support economic competitiveness, scientific research and education, and push the boundaries of fundamental knowledge. The caucus has asked NUFO to present this message during a caucus event on Capitol Hill, which may be held in early June 2013. The NUFO Steering Committee selected the title "Discoveries that Improve Your Life: National Research Facilities Tackle Grand Challenges" with theme areas of health, energy, and transformational technologies as the centerpiece of this science exhibition.

Argonne's Nanoscience Program Restructured

Effective December 3, 2012, Argonne has a new division, Nanoscience and Technology (NST), which contains two user facilities: the Center for Nanoscale Materials and the Electron Microscopy Center. There are no operational or organizational changes within the user facilities as a result of the new name.

Argonne Gets $120M for New Batteries and Energy Storage Hub

The U.S. Department of Energy (DOE) Office of Science awarded Argonne up to $120M to establish the Joint Center for Energy Storage Research (JCESR). This exciting scientific venture is focused on invention, innovation, and commercialization of revolutionary energy storage technologies with a goal of "Five-Five-Five" — creating batteries that are five times more powerful and five times less expensive within five years. In addition to Argonne, the partners include four national laboratories, five universities, and three industrial partners. The Clean Energy Trust is also involved. (Read the DOE news release and additional articles here and here.)

Congress Highlights U.S. Investment in Research: The Year of the Federal Lab

Randy Hultgren (R-IL-14) and Chaka Fattah (D-PA-02), a senior member of the House Appropriations Committee, introduced legislation to focus on the critical U.S. investment in research by declaring 2013 the "Year of the Federal Lab." On November 16, House Resolution 815 was introduced, which states that federal laboratories have been and continue to be at the cutting edge of scientific and technological advancement. (Read press release published on Congressman Hultgren's web site.)

User Notes

Acknowledgment of the use of DOE user facilities in scientific publications and technical presentations is vital for their future sustainability. An acknowledgment statement must be included in all published reports of work conducted at CNM. (Review the guidance.)

We are excited to chronicle the scientific advancements of CNM's users by your user activity reports. Since time is becoming more competitive, completion of reports on past projects is now required for consideration of new proposals.

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Probing Picasso's Paints with the Hard X-Ray Nanoprobe

Scientists from the Art Institute of Chicago, together with the X-Ray Microscopy Group, have exploited the Hard X-Ray Nanoprobe's high-resolution X-ray fluorescence (XRF) mapping capability for the analysis of artists' paints. By analysis of the metal impurities (lead, cadmium, iron, etc.) in zinc oxide pigments used in early 20th Century artists' paints, it was proven that Pablo Picasso and his contemporaries used the highest quality, nearly pure, zinc oxide pigments. This pigment was present in Ripolin, a popular brand of French house paint, as by far the major ingredient. Nanoprobe XRF mapping also demonstrated that most artists' tube paints have more fillers and additional whites (based on lead, titanium, and calcium) than Ripolin. The nanoprobe's high spatial resolution and microfocusing abilities allowed it to peer deeper than previous studies, which were limited to micrometer resolution, for an unprecedented look at 30-nm particles of paint. The chemical characterization of paints at the nanoscale opens a path to better understanding their fabrication and reactivity.

Picasso: The Red Armchair

Picasso used Ripolin commercial house paint in this work, The Red Armchair (1931).

F. Casadio and V. Rose, "High-resolution fluorescence mapping of impurities in historical zinc oxide pigments: hard X-ray nanoprobe applications to the paints of Pablo Picasso," Appl. Phys. A., 2013 (online)

Atomistic Simulations of Battery Materials

The experimental and theoretical work of users from the University of Chicago, together with the Nanobio Interfaces and Theory & Modeling Groups, shows a strong correlation between the structural stability of cubic titania nanotubes and the concentration of intercalated lithium ions in a new class of battery materials that display exceptionally high specific power while retaining high specific energy upon cycling. Theoretical calculations based on classical molecular dynamics demonstrate a unique atomistic scale response mechanism in which cation intercalation induces remarkable stability of defective materials under an applied stress. The associated enhancement in structural stability arises from a vacancy filling mechanism in which an applied pressure drives interstitial lithium ions to vacancy sites in the oxide interior. This study provides fundamental insights into the correlation between the structure and function of materials used in energy storage applications. The results are of significance to understanding mechanisms of structural response of metal oxide electrode materials at high pressures as well as emerging energy storage technologies utilizing such materials.

H. Xiong et al., "Compositional Tuning of Structural Stability of Lithiated Cubic Titania via Vacancy Filling Mechanism under High Pressure," Phys. Rev. Lett., 110, 078304 (2013). (abstract)

Atomistic simulation of battery materials

Computational predictions of structural transitions for charged, delithiated (top) and discharged lithiated (bottom) c-TiO2 nanotubes under high pressure; red sphere = O; green = Li; white = Ti.

Enhanced Light Harvesting in QD-MOF Assemblies

Users from Northwestern University, working together with the Nanophotonics Group, have reported the functionalization of porphyrin-based metal-organic frameworks (MOFs) with CdSe/ZnS core/shell quantum dots (QDs) for the enhancement of light harvesting via energy transfer from the QDs to the MOFs. Because of their efficient energy-transport properties, porphyrin-based MOFs are attractive compounds for solar photochemistry applications. However, their absorption bands provide limited coverage in the visible spectral range for light-harvesting applications. The broad absorption band of the QDs in the visible region offers greater coverage of the solar spectrum by QD-MOF hybrid structures. Time-resolved emission studies at CNM show that photoexcitation of the QDs is followed by energy transfer to the MOFs with efficiencies of more than 80%. This sensitization approach can result in a >50% increase in the number of photons harvested by a single monolayer MOF structure with a monolayer of QDs on the MOF surface.

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Quantum dot metal organic framework

Schematic of a QD-MOF complex; QDs are 5-6 nm. The MOF is a small region of a larger planar structure; the interporphyrin spacing is about 1 nm. Excitons can migrate at least 10 layers (15 nm).

S. Jin et al.,"Energy Transfer from Quantum Dots to Metal-Organic Frameworks for Enhanced Light Harvesting." J. Am. Chem. Soc.,135, 955 (2013) (doi)

Kurt Lesker Sputtering Deposition and Electron-Beam Evaporation System

The Kurt Lesker sputtering deposition and electron-beam evaporation system, managed by Electronic & Magnetic Materials and Devices (EMMD), is housed in the clean room facility of the CNM. This versatile tool offers sputtering and e-beam evaporation capabilities for depositing a wide variety of polycrystalline and amorphous films onto substrates up to 6 inches in diameter. A common load-lock assembly and robotic arm allows sample transfer from one system to the other without breaking vacuum.

  • The sputtering CMS18, with pressures between 10-8 and 10-10 Torr, contains one radio-frequency and four direct current magnetron guns in a confocal arrangement with standard and high-strength magnetic field configurations, mass flow controllers, substrate rotation, and heater (up to 850°C).
  • The e-beam PVD250, with pressure in the 10-8 and 10-9 Torr range, is equipped with a 10-kW four-pocket electron gun. Wafer biasing (100 W, RF) can be used to eliminate resist exposure from secondary electrons. A water chiller keeps substrates and QCM heads at room temperature, resulting in smooth, controlled evaporation.

The capabilities of the Lesker tool will soon be expanded even further. The power will be increased up to 20 kW with up to eight different sources, allowing for the sequential evaporation of a larger number of multilayers as well as co-evaporated materials (alloys).

Examples of the many diverse applications to which the Lesker tool has contributed include epitaxial films (gold, chromium); ultrasmooth films (gold, silver) for solar cell and plasmonic applications; high-quality superconducting films (aluminum, niobium, tantalum, and tungsten silicide) for optical/ultraviolet microwave kinetic inductance detector-based X-ray detectors), ferromagnetic/superconducting hybrids, and the development of smart-tips for high-resolution microscopy. For more information contact Dan Rosenmann.

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Lesker Tool

Lesker Tool: sputtering and e-beam evaporator with common load-lock

Magnetization vs temperature of niobium superconducting films

Magnetization vs. temperature of niobium superconducting films

T Cecil et al., "Tungsten Silicide Films for Kinetic Inductance Detectors," Appl. Phys. Lett. 101, 032601 (2012)

Tijana Rajh

Tijana Rajh, NanoBio Interfaces Group Leader, was among the 14 Argonne employees selected by Argonne's director to participate in the 2012 Strategic Laboratory Leadership Program. Candidates in the program are individuals who show leadership abilities, exceptional work ethic, collaborative thinking skills, rigorous scholarship aptitude, and innovative and creative problem-solving capabilities. Seventy-five candidates from Argonne have participated in this program since 2007. The program provides conceptual tools to manage complex projects in a practical, real-world scenario. UChicago Argonne, LLC, sponsors the non-degree executive leadership program developed by the Chicago Booth School of Business for the programmatic and operations staff of Argonne and Fermilab.

Adina Luican-Mayer

Adina Luican-Mayer joined the Electronic & Magnetic Materials & Devices Group in September 2012 as Argonne's Alexei Abrikosov Named Postdoctoral Fellow. Her general research interests include studying low-dimensional systems, such as graphene or graphene-based materials, by using combined local probe techniques and electrical transport. She is working with Nathan Guisinger on understanding the unique nature of charge carriers in graphene via scanning tunneling microscopy and spectroscopy at low temperatures and in magnetic fields.

Jeff Greeley

Jeffrey Greeley recently transitioned to the School of Chemical Engineering at Purdue University as an associate professor. His research interests are in the area of first principles theories of interfacial science and catalysis. Jeff was the recipient of a DOE Early Career Award in 2011 while at CNM, and he retains a guest appointment at CNM in the Theory & Modeling Group.

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