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

Amanda Petford-LongAs I write to you in early June, the CNM is in the process of preparing for our triennial DOE Basic Energy Sciences (BES) review this August. I am impressed by the incredibly high standard of user projects taking place at the CNM, and I am grateful to all of you who contribute highlights that we can include. At the onsite review, we will host a poster session featuring both user and staff research, and I hope that you will consider making yourselves available to support CNM in this important activity if called upon.

In late February, a subcommittee of the DOE-BES Advisory Committee was charged with reviewing the BES scientific user facilities and producing a facilities prioritization report. We are pleased to say that the CNM was placed in the highest category, namely "absolutely central," to world-leading science for the period 2014 to 2024. The full report of the committee is publicly available. In April, we welcomed our new Scientific Advisory Committee (SAC) to CNM. Together with the Users Executive Committee and the Proposal Evaluation Board, the SAC help the CNM to remain committed to a very high level of science, and we are extremely grateful for their support.

The high point of the last few months at the CNM was the Argonne Users' Meeting, which was held in May and attracted over 500 participants. The CNM, APS, and EMC jointly organized successful cross-cutting symposia, and the meeting included our own CNM workshop and short courses. An inaugural satellite workshop was held for the industrial community, jointly organized with the APS, which attracted participants from 15 companies. As always, one of the most enjoyable parts of the meeting for me was the poster session, which allows the opportunity to get a more detailed insight into the exciting range of science that our users are carrying out at CNM.

The week following the Users' Meeting was one of our planned maintenance periods. Preventive maintenance on a number of user program capabilities was performed as well as an upgrade to the gas alarm system software for the cleanroom. CNM staff members have been very active collectively, giving invited talks at conferences and taking part in myriad outreach activities. Several were recently recognized with prestigious awards; please read the details further in this newsletter and join me in congratulating them for their well-deserved recognition.

Finally I would like to offer a welcome to our summer student and faculty visitors who have arrived and become an integral part of our user community. I encourage everyone to scan the various facility and user science highlights, staff news, and important user matters that are included in this issue of nanoMATTERS. Enjoy a safe and productive summer.

Amanda Petford-Long, CNM Director

Call for Proposals Deadline: July 12, 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

Over 530 registrants, plus an additional 100 vendors from 55 exhibitor booths, participated in the wide array of activities available at this annual showcase event. Cross-facility, thematic workshops on batteries, imaging, and "big" data management highlighted, promoted, and stimulated user science from the CNM, the Advanced Photon Source, and the Electron Microscopy Center. The CNM plenary session kicked off with a keynote address by Paul Nealey of the University of Chicago and continued with several CNM user science highlights. There also was a CNM facility-specific workshop on "Nanostructured Carbon Materials for MEMS/NEMS and Nanoelectronics," the largest-ever poster session, a vendor expo, CNM short courses, and social events. The CNM Best Student Poster prize winner was Mark Huntington (Northwestern University). Meeting details and photos are available online.

Users Executive Committee Updates

The CNM Users Organization recently voted to accept a revised set of Users Executive Committee (UEC) by-laws. The UEC will increase from six to nine members over the course of three years, which will allow greater and more diverse representation of the ever-growing CNM user community. The three newly elected UEC members are Matthew Grayson (Northwestern University), Axel Hoffmann (Argonne), and Steve Smith (South Dakota School of Mines and Technology). Completing their terms were Kristen Buchanan (Colorado State University) and John Freeland (Argonne). As past chair, John remains as an ex officio member. The current chair is Steven May (Drexel University), and the vice-chair is Seungbum Hong (Argonne).

Workshop on User Facilities for Industry 101

Several industrial scientists and engineers attended 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. The successful workshop showcased several successful industrial user experiments and explained the different ways in which industrial scientists can work with Argonne scientists. Representatives from Argonne's user facilities as well as from the Technology Development and Commercialization Division were available to discuss the feasibility of research ideas and the various modes available for accessing the facilities. The workshop concluded with facility tours that gave participants the opportunity to interact directly with scientists.

NUFO Science Exhibition on Capitol Hill: June 26, 2013

In response to an invitation from the House Science and National Labs Caucus, the National User Facility Organization (NUFO) will hold a science exhibition in the Gold Room of the Rayburn Office Building on Wednesday, June 26, 2013. Hands-on demonstrations, videos, and posters in the areas of health, innovation, and energy will showcase the accomplishments of NUFO users, as well as provide insights on NUFO's role in educating the next-generation scientific workforce. Brief remarks by members of Congress, representatives from industry, the DOE Office of Science, and national laboratory management will highlight the role of user facilities in America's scientific infrastructure. CNM user Adam Khan of AKHAN Technologies and his collaborator, CNM staff member Ani Sumant, are attending the event to present a demonstration on energy-efficient nanoelectronics. Another exhibit will contain a video featuring user projects with the NanoBio Interfaces Group. See the May 2013 issue of NUFO News if you would like to participate in the exhibition.

Summer Lab Attire

Now that the summer months are upon us, it's a good time to remind everyone of appropriate lab attire. Recall that in the laboratory wing, sandals, shorts, and sleeveless tops are not allowed. Please plan accordingly, e-mail any questions to the CNM User Office, and have a safe and successful laboratory experience.

CNM Closed to Users September 2-8, 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 user activities. These periods, lasting 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.

From September 2-8, 2013, users are not allowed to work in CNM laboratories in Buildings 440 and 441, nor will they able to access the Carbon high-performance computing cluster. The closure dates include the Labor Day holiday and the following weekend. The CNM will reopen to users on Monday, September 9. Please plan your work visits and schedules accordingly.

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 highlights. Since time is becoming more competitive, submission of highlights on past projects is now required for consideration of new proposal allocations.

Nanomechanical Resonator Self-Assembled from Nanoparticles

The self-assembly of nanoscale structures from functional nanoparticles has provided a powerful path to developing devices with emergent properties from the bottom up. Users from the University of Chicago, together with researchers from the University of Melbourne and CNM's Electronic & Magnetic Materials & Devices Group, demonstrate that free-standing sheets self-assembled from various nanoparticles form versatile nanomechanical resonators in the MHz frequency range. Using spatially resolved laser interferometry to measure thermal vibrational spectra and image vibration modes, they show that the resonator's dynamic behavior is in excellent agreement with linear elastic response for prestressed drumheads of negligible bending stiffness. Fabricated in a simple one-step drying-mediated process, these resonators are highly robust, and their inorganic-organic hybrid nature offers an extremely low mass, low stiffness, and the potential to couple the intrinsic functionality of the nanoparticle building blocks to nanomechanical motion.

P. Kanjanaboos et al., "Self-Assembled Nanoparticle Drumhead Resonators," Nano Lett., 13, 2158 (2013).

Power spectral distribution

Power spectral distribution of the thermal motion of membranes self-assembled from gold nanoparticles taken at the center (black) and halfway along the radius (red) in air; inset shows TEM images of the membranes

Phase-sensitive image

Phase-sensitive image of one mode of membrane motion under mechanical excitation

Imaging Nanoscale Polarization in Ferroelectrics with Coherent X-Rays

Users from Argonne's Materials Science and Nanoscience & Technology divisions, in collaboration with CNM's X-Ray Microscopy Group and researchers from the Advanced Photon Source, KAIST, Northern Illinois University, and the University of Melbourne, used the new X-ray imaging technique of coherent X-ray Bragg projection ptychography for the study of nanoscale structures in ferroelectric thin films. Under certain conditions, ferroelectric thin films (used, for example, in specialized computer memories) form networks of nanoscale domains with distinct local polarizations that are difficult to image because their properties are controlled by the film's surrounding environment. Noninvasive visualization of these polar domains under realistic boundary conditions is key to the continued development of ferroelectric devices. The Bragg ptychography method employs a highly penetrating nanofocused X-ray beam to create spatially overlapping coherent diffraction images, which, in this study, were used to visualize nanoscale domain polarization in an epitaxially strained ferroelectric thin film of PbTiO3. With a demonstrated spatial resolution of less than six nanometers, this new quantitative imaging technique has paved the way for the visualization of domain morphology and behavior inside ferroelectric heterostructures under relevant conditions.

S. O. Hruszkewycz et al., Phys. Rev. Lett., 110, 177601 (2013).

Local polarization in ferroelectric thin film

Quantitative images of local polarization in a PbTiO3 ferroelectric thin film as imaged with Bragg projection ptychography (a) and with piezoresponse force microscopy (b) at respective spatial resolutions of 5.7 and 22 nm.

Tuning the Catalytic Activity of Ru@Pt Core-Shell Nanoparticles

Users of the Theory & Modeling Group's high-performance computing cluster Carbon from the University of Wisconsin-Madison, and their collaborators, investigated the kinetics of the oxygen reduction reaction (ORR) in acid solutions on platinum (Pt) monolayers that were deposited on carbon-supported ruthenium (Ru) nanoparticles. The Pt mass and specific ORR activities were found to greatly depend on the number of Pt monolayers, and the optimum activity occurs with two Pt monolayers. Density functional theory calculations showed that Pt overlayers destabilize O* and OH* with respect to pure Pt, leading to more favorable hydrogenation kinetics. However, with only a single Pt overlayer, the destabilization is too great and O-O bond breaking becomes rate limiting. This work demonstrates that ORR activity of Pt monolayers supported on other metals can be modulated by eliminating a part of the ligand effect by increasing the thickness of the Pt shell on top of the supporting metal surface.

L. Yang et al., " Tuning the Catalytic Activity of Ru@Pt Core-Shell Nanoparticles for the Oxygen Reduction Reaction by Varying the Shell Thickness," J. Phys. Chem. C, 117, 1748 (2013)

Ru-Pt Core-Shell Nanoparticles

Renishaw inVia Raman Microscope

The Nanophotonics Group’s Raman microscope was recently upgraded with a new high-resolution camera and transmission dark-field viewing capability. The 3-megapixel camera is fully integrated into the microscope's software allowing for high-quality optical images to be overlaid with confocal Raman data. Full dark-field capability is planned; transmission mode is available, and reflection mode is planned for later this year.

The Raman microscope is a versatile tool for Raman spectral measurements on a wide variety of samples. Laser excitation is available at five wavelengths: 325, 442, 514, 633, and 785 nm, which means that fluorescence backgrounds can almost always be avoided. The availability of many excitation wavelengths also allows for specialty techniques, such as resonance and surface-enhanced Raman spectroscopy. Switching between wavelengths takes less than five minutes, and the system also auto-aligns and auto-calibrates. The microscope provides fully automated X-Y area mapping with submicron spatial resolution. Additional add-ons allow for macro sampling from vials, cuvettes, NMR tubes, etc. The temperature-controlled microscope stage is programmable from 77 to 800 K. Integrated software seamlessly controls programmable temperature ramps and the acquisition of spectra.

The Raman microscope has been used to examine samples ranging from carbons, such as nanotubes, ultrananocrystalline diamond, fullerenes, and graphene, to battery cathode materials, and self-assembled three-dimensional nanocrystals.

Contact David Gosztola of the Nanophotonics Group for more information.

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Raman Microscope

Raman microscope

Two-dimensional peak mapping of graphene

Triobological test of graphene

Two-dimensional peak mapping of graphene layers during tribological tests. [Berman et al., Carbon, 59, 167 (2013)].

Gary Wliederrecht

Gary Wiederrecht, Group Leader of the Nanophotonics Group, is a 2013 Distinguished Performance Award recipient. This award is given by the UChicago Argonne, LLC, Board of Governors of Argonne National Laboratory. Distinguished Performance Awards recognize the outstanding scientific or technical achievements, or a distinguished record of achievement, of select Argonne employees. Gary will be honored in an awards ceremony and reception on Thursday, August 15, 2013, in the Building 402 conference center.

Elena Rozhkova

Elena Rozhkova, Nanobio Interfaces Group, shares a 2013 Distinguished Performance Award with Val Novosad of Argonne's Materials Science Division. This award is given by the UChicago Argonne, LLC, Board of Governors of Argonne National Laboratory. Distinguished Performance Awards recognize the outstanding scientific or technical achievements, or a distinguished record of achievement, of select Argonne employees. Elena and Val will be honored in an awards ceremony and reception on Thursday, August 15, 2013, in the Building 402 conference center.

Marcia Wood

Marcia Wood, Group Leader of the Computing & Information Technology Group, is a 2013 Outstanding Service Award recipient. This award is given by the UChicago Argonne, LLC, Board of Governors of Argonne National Laboratory. Outstanding Service Awards recognize employees in support positions who have furthered Argonne's goals and missions through their exceptional contributions during their careers at the Laboratory. Marcia will be honored in an awards ceremony and reception on Thursday, August 15, 2013, in the Building 402 conference center.

Andreas Roelofs

Volker Rose

Andreas Roelofs, CNM Deputy Director and Industrial Liaison (NST), (top), and Volker Rose, X-Ray Microscopy Group and Advanced Photon Source, (bottom), were among the 15 Argonne employees selected by Argonne's director for the 2013 Strategic Laboratory Leadership Program (SLLP). 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. 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, Fermilab, Jefferson Lab, and the University of Chicago.

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