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

Amanda Petford-LongGreetings to all from a snowy, cold Chicago. Our facilities group was very busy ensuring that the infrastructure across CNM remained operational during the extremely cold weather at the start of January, which in fact even led to the closure of Argonne Laboratory for a few days.

The CNM has been quite busy for the past several months, including our triennial review held last August. I extend my sincere gratitude to all of the users who participated. Several of our users presented posters to the review committee or met with the reviewers over lunch along with the Users Executive Committee. We were delighted that Venkat Gopalan, Libai Huang, Adam Khan, and Claire Xiong were able to present user highlight talks. I know that taking part in an activity of this nature is time-consuming, and I was very impressed by the level of commitment that our user community showed towards CNM.

A big change that will occur this year is the addition of the Electron Microscopy Center into the CNM as a seventh group. We are very excited about this development because of the many synergies between the CNM and EMC science programs. Additionally, we believe that this will greatly enhance the experience for both CNM and EMC users, since all capabilities will now appear within the CNM user proposal form in one unified system. The March Call for Proposals will be the first for which the combined capabilities will be available, and we welcome your feedback on how this works.

The budget situation this year is challenging, but we are doing our best to ensure that we keep all capabilities at CNM open to our user community and that user needs are met. Indeed we have installed a number of new capabilities since the end of fiscal year 2013, including a new scanning electron microscope for the cleanroom, a gas reaction cell holder for the TEM, and an accessory for the UV-VIS-NIR spectrometer.

On the staffing front, we recently welcomed Julie Emery as User Program Administrator and David Eckstein as a Principal Applications Developer. Please join me also in congratulating Tijana Rajh on being made a Fellow of the AAAS, Ani Sumant on being awarded two R&D100 awards (one of which is connected with his work at CNM), Gary Wiederrecht and Elena Rozhkova on their University of Chicago Outstanding Performance Awards, and Marcia Wood for her Outstanding Service Award from the University of Chicago. CNM staff are again providing lectures at Northwestern University as part of a graduate program on nanomaterials. The class was received well by the students at Northwestern last year, and so we were invited back for a repeat performance. I am grateful for the time that CNM staff are committing to this outreach activity.

I hope that 2014 will be a very successful year for everyone and I look forward to welcoming you to CNM.

Amanda Petford-Long
CNM Facility Director

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Call for Proposals Deadline: March 7, 2014

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

Note two changes with this call:

  1. There is a new look and feel with some of the proposal web form's functionality.
  2. There are additional electron microscopy capabilities as a result of the incorporation of the Electron Microscopy Center as a new research group within CNM.

(More >>)

CNM Users Meeting, May 12-15, 2014

The annual combined APS/CNM/EMC Users Meeting will be held May 12-15, 2014, at Argonne National Laboratory. More than 500 people register for these cross-cutting meetings, which include 40-50 vendor exhibits, workshops, poster sessions, and short courses. Anyone is welcome to register.

Thematic and facility-specific workshops will highlight, promote, and stimulate user science from these premier user facilities. The CNM Plenary Session will feature a keynote presentation by Prof. Federico Capasso of Harvard University. The energy-focused cross-facility workshop is "Beyond Lithium Ion Batteries: Chemistry, Materials, and Characterization," and the CNM workshop is "Solar Energy Capture and Conversion at the Nanoscale."

Check the meeting website for deadlines and the CNM Events page for programming updates.

CNM News & Science Highlights

Interested in the latest nanotech advances regarding historical preservation or cultural heritage? Your interests lie in nanobio health and medical applications, solar energy, nanomechanical resonators, or ferroelectrics? This list of fascinating nanoscience developments at the CNM goes on and on. Since these triennial issues of nanoMATTERS can't keep up with the fast pace of our science & technology breakthroughs, bookmark the CNM web site, Like Us on Facebook, and peruse the lists of breaking News and Research Highlights to keep up with us!

NUFO Goes to Capitol Hill

NUFO has begun planning the 2014 Facility Science Exhibition for the U.S. House of Representatives, which is anticipated to take place in June 2014. This year's themes are Discovery and Energy. The format will be similar to that of the 2013 NUFO exhibition. Preliminary information on the exhibition is available online.

"Get Your Geek On" was the call issued by Congressman Randy Hultgren's office to the House of Representatives about the 2013 National User Facility Organization (NUFO) User Science Exhibition on Capitol Hill on June 26, 2013. The exhibition focused on the themes of energy, health, and innovation. Among many demos were three spin-off products from discovery research at user facilities, including AKHAN Technologies' nanocrystalline diamond coatings together with CNM (see below for Award news regarding this technology). Posters highlighted the faces and places of science, science and technology education initiatives, and user accomplishments. Comments from Congressmen Chaka Fattah and Randy Hultgren emphasized the importance of user facilities and our national laboratories in America's scientific infrastructure, while Harriet Kung, Director of the DOE Office of Basic Energy Sciences, spoke of "partnering with NUFO" to get the word out about critical science discoveries. Read more on the NUFO web site.

CNM Closure: April 28-May 4, 2014

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 approximately 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 undergo preventive maintenance that will help avoid unplanned shutdowns. The annual maintenance period schedule is available online.

The next CNM preventive maintenance period will be in effect from April 28-May 4, 2014, inclusive of the weekend. During this time, the CNM will not be available for user activities in laboratories or on the High-Performance Computing Cluster; however, administrative support will be available. User activities resume on Monday, May 5, 2014. Please plan your work visits and schedules accordingly.

CNM Data Management Practices

CNM is committed to providing our users with their data in a timely and convenient fashion. CNM users, however, are responsible for meeting their data management obligations to their home institutions and funding agencies. The CNM does not provide long-term data archiving or management service. CNM facility users who generate and store data on CNM-owned equipment have 30 days from the expiration of the relevant user work approval document to copy or move their data to non-CNM-owned equipment. After that time, the CNM may delete the data, including backups, from CNM-owned equipment. If you have questions or concerns about this policy then please contact the CNM User Office.

U.S. Congress Acts to Avert Helium Shortage

The U.S. Congress passed legislation in Fall 2013 that prevents a market shortage of helium. The Federal Helium Program, operated under the Bureau of Land Management, supplies some 42% of the helium gas used in the United States. The closure had been planned for October 7 when the government would have been required to end helium sales to the private sector, which has yet to develop sufficient infrastructure production and could have faced a surge in prices. Several industrial and university researchers started a campaign to lobby Congress about the need to change course. The bill provides for continuation of helium sales by auction until the reserve is gradually depleted. (More >>)

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.

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Thermotropic Phase Boundaries in Classic Ferroelectrics

Novel monoclinic subphases in ferroelectric BaTiO3 were observed by users from The Pennsylvania State University in collaboration with CNM's X-Ray Microscopy Group and Oak Ridge National Laboratory's Center for Nanophase Materials Sciences. The new low-symmetry intermediate phases are locally stabilized near thermotropic phase boundaries in simple ferroelectrics and exhibit large enhancements in nonlinear optical and piezoelectric property coefficients. This discovery presents unique opportunities for the design of "green" high-performance nanoscale energy materials. The findings reveal that phase transitions in ferroelectrics are intimately coupled to the underlying domain microstructure. Even in lead-free BaTiO3 and KNbO3, classic materials that have been known and studied for more than 60 years, this new observation shows that domains can lend a thermotropic character to their otherwise well-known phase transitions. This leads to the emergence of intermediate monoclinic phases in a wide temperature range around the conventional interferroelectric transitions. Nanoscale scanning X-ray diffraction measurements harnessing the unique structural sensitivity of the CNM Hard X-Ray Nanoprobe unambiguously demonstrated the intrinsic monoclinic nature of the subphase.

T. A. Lummen et al., Nat. Commun, 5, 3172 (2014); doi:10.1038/ncomms4172

Orthogonally Twinned BaTiO3

Scanning hard X-ray diffraction image (aspect-ratio-corrected spatial map) of the (220) Mc peak intensity in orthogonally twinned BaTiO3 (scale bar 10 µm)

Black Tungsten for Solar Power Generation

The viability of nano-textured tungsten as an efficient solar absorber has been explored via computational electrodynamics simulations by users from the University of Virginia, working with CNM's Theory & Modeling Group. The researchers show that sunlight absorption over 99% can be achieved by using pseudo-random nanostructured tungsten. The nanostructure remains highly absorbing in the solar spectrum over a large temperature range. The use of protective oxide coatings further enhances the solar absorption and is dependent upon their thickness. The oxide layer provides protection from oxidation at high operating temperatures. The aperiodic nature of this surface also allows for relaxed fabrication requirements, leading to lower cost designs. The availability of an easy-to-manufacture surface with high solar absorption and high temperature stability may have significant impact on solar thermal and solar thermophotovoltaic applications. The relaxed manufacturing requirements for pseudo-random surfaces represent a significant cost savings to the industry as well.

C. Ungaro, S. Gray. and M.C. Gupta, Appl. Phys. Lett., 103, 071105 (2013)

Simulated reflectanct of oxides on a tungsten substrate

Simulated reflectance for different thicknesses of oxides on a textured tungsten substrate. The cone average radius = 500 nm, FWHM = 300 nm, 95% of the substrate is filled with cones.

Extreme Confinement of Electromagnetic Waves

Squeezing light through nanometer-wide gaps in metals can lead to extreme field enhancements, nonlocal electromagnetic effects, and light-induced electron tunneling. This intriguing regime, however, has not been readily accessible to experimentalists because of the lack of reliable technology to fabricate uniform nanogaps with atomic-scale resolution and high throughput. Users from the University of Minnesota, working with the CNM's Nanophotonics Group and Seoul National University, have introduced a new patterning technology based on atomic layer deposition and planarization. Vertically oriented gaps in opaque metal films were created along the entire contour of a millimeter-sized pattern, with gap widths as narrow as 9.9 angstroms; 150,000 such devices were packed on a 4-inch wafer. Electromagnetic waves pass exclusively through the nanogaps, enabling background-free transmission measurements. Resonant transmission through 1.1-nm-wide gaps was observed for (a) near-infrared waves (lambda/1,295), and (b) millimeter waves (lambda/4,000,000), revealing an unprecedented field enhancement factor of 25,000.

X. Chen, et al., Nature Comm., 4, 2361 (2013)

Transmission spectra

Transmission spectra at near-infrared wavelengths through a 1.1-nm gap in a 190-nm-thick gold film (red) and a 2-nm-gap in a 200-nm-thick gold film (black). Numbers are the mode orders of Fabry-Perot resonances in the nanogap waveguides.

Geometrically Frustrated Ice State in Nanopatterned Superconductors

Geometrical frustration, a broad phenomenon occurring in many areas of condensed physics, arises from an intrinsic incompatibility between fundamental interactions and an underlying ordered lattice structure. Recent work studied the transport properties of MoGe thin films with a special arrangement of holes, which allows the formation of a geometrically frustrated vortex ice state. These vortex ices, which are an entirely new artificial ice system, allow electrical transport measurements that are not easily accessible in other ice systems. The research team used focused-ion-beam (FIB) lithography and laser writer patterning in CNM’s Nanofabrication & Devices Group to create the ice systems. The convenience in creating vacancies or interstitials that locally break ice rules by changing the applied magnetic field enables the vortex ice to be an excellent platform for the investigation of defect formation processes. Ginzburg-Landau numerical simulations demonstrated that the enhancement of the critical current, observed near the half-matching field over a broad temperature range, is closely related to the vortex arrangements in the system, confirming the vortex-ice ground state.

M.L. Latimer et al., Phys. Rev. Lett. 111, 067001 (2013).

Critical current vs magnetic field for vortex ice

Critical current Ic vs. magnetic field at T = 4.8 and 4.9K

SEM of vortex ice sample

SEM of sample; hole diameter a = 102 nm, interhole spacing d = 300 nm, H1 = 156 Oe is the first matching field

Multiexciton Solar Cells of CuInSe2 Nanocrystals

Transient absorption spectroscopy at CNM played a critical role in the detection of multiexcitons in the inexpensive model thin film semiconductor CuInSe2. Users from the University of Texas at Austin, working with the Nanophotonics Group, together developed this new, inexpensive material that has the potential to capture and convert solar energy, particularly from the bluer part of the spectrum, more efficiently. CuInSe2 is closely related to another more commonly produced thin film that holds the record for the most efficient thin-film semiconductor, CIGS (a CuInGaSe2 material). In order to deposit thin films of the nanocrystalline material, "photonic curing" was used, which involves quickly heating up and cooling down of the top layer of the material. This curing process not only prevented the melting of the glass that contains the nanocrystals, but also vaporized organic molecules that inhibit multiple exciton extraction.

C. J. Stolle et al., J. Phys. Chem. Lett. 5, 304 (2014).

Photonic curing process of nanocrystals

Photonic curing process schematic of the approximately 8-nm CuInSe2 nanocrystals.

Omicron VT-UHV SEM/SAM/SPM Four-Probe Station

The Omicron UHV probe station within the EMMD Group provides scanning electron microscopy (SEM) with scanning Auger analysis and mapping (SAM), and scanning tunneling microscopy (STM)-based four-probe analysis capabilities. The UHV Gemini electron microscope furthermore provides SEM imaging and enables precise positioning of the four independently controlled STM tips. Two of these STM tips can be used to acquire STM imaging, thereby allowing investigations of the sample surface locally. The system has a variable-temperature sample analysis stage controllable from 40 to 650 K.

Keithley meters and custom LabVIEW programs are equipped for electrical characterization, including I-V curves and electromigration measurements. The electronics of the system consist of a sub-femtoamp source meter, nanovoltmeter, and electrometers. Moreover, the UHV system has an integrated sample preparation chamber with sample heating and sputtering, low-energy electron diffraction, and Auger electron spectroscopy for sample analysis and e-beam evaporators for material depositions. The samples can be grown in the prep chamber and transferred to the SEM/STM analysis chamber without exposure to the atmosphere.

CNM's Omicron UHV system has been used to characterize novel batteries and ultrananocrystalline diamond materials; for testing MEMS devices; and for in situ deposition of metallic, bimetallic, and metal-silicide nanowires and nanorods.

Contact Brandon Fisher of the EMMD Group for more information.

Omicron VT-UHV sample stage

Side view of the Omicron SEM/STM sample stage showing SEM and STM tips

lead sulphide superlattices

Self-assembled three-dimensional periodic superlattices from lead sulfide showing two STM tips. The entire image scale is 4 x 4 µm (P. Podsiadlo, N. Kotov, unpublished results)

Tijana Rajh

Tijana Rajh, Leader of the Nanobio Interfaces Group, was named a Fellow of the American Association for the Advancement of Science (AAAS) in November 2013. Tijana was elected for her "distinguished contributions to the fields of nanoscience and nanotechnology, with particular emphasis on semiconductor-assisted photocatalysis, solar energy conversion and energy storage." Rajh earned her doctorate from the University of Belgrade in Yugoslavia; she is a prolific researcher, co-authoring more than 150 papers and holding four patents.

Ani Sumant

Ani Sumant's (Nanofabrication & Devices Group) involvement in two 2013 R&D 100 awards make him the first Argonne researcher to win two of the awards in the same year. One, the Miraj Diamond Platform, consists of the combination of two new diamond technologies: low-temperature nanocrystalline diamond deposition developed at CNM and an efficient n-type semiconductor doping process developed by industrial user AKHAN Technologies. The other was for co-developing a nanocrystalline diamond coating for micro-tools before joining CNM.

Subramanian Sankaranarayan

Subramanian Sankaranarayanan (Theory & Modeling Group) received a 2014 Innovative and Novel Computational Impact on Theory and Experiment (INCITE) award. As the principal investigator for "Reactive MD Simulations of Electrochemical Oxide Interfaces at Mesoscale," with co-investigators from Harvard University and the University of Missouri-Columbia, he was awarded 40,000,000 processor hours on Argonne's IBM Blue Gene/Q "Mira." The award duration is for three years pending annual review.

Julie Emery

Julie Emery Collins joined the CNM User & Outreach Programs Office as the new User Program Administrator in late July, replacing Carrie Clark who left Argonne to pursue a small business venture. Julie has an exemplary record of customer service, having served as the executive secretary for 12 years in Argonne's Materials Science and Chemistry divisions. Her many years of experience with Argonne's various business systems and onboarding new employees have prepared her well for this new role.

David Eckstein

David Eckstein joined the Computing and Information Technology group as a Principal Application Developer in July 2013. David has spent nearly 20 years in the IT field, with roles in desktop and server support, networking, and software development. As a contractor to the CNM for the past six years, David has developed all the user program's database applications that are in use at the CNM today.

Jun Suk Rho

Jun Suk Rho, Argonne Ugo Fano Named Postdoctoral Fellow, joined the Nanofabrication & Devices Group in August from the University of California at Berkeley. Jun's research is focused on developing novel metamaterials and plasmonic materials based on fundamental physics and experimental studies of deep subwavelength nanophotonics. Device applications include superresolution imaging, optical cavities, negative index materials, metasurfaces, and nanolaser and sub-10-nm nanolithography.

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