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6
Surface and Microanalysis Science Division
SUMMARY
The mission of the Surface and Microanalysis Science Division (SMSD) is to serve
the nation in areas of chemical metrology, research, standards, and the acquisition and
analysis of data. The SMSD provides excellent service to the U.S. government and the United
Nations through the identification of radioactive and explosive materials as well as the setting
of sample standards and development of analytical methods. SMSD research includes a wide
range of topics that are critical to the maintenance of national standards and measurement
science for the nation. The division is well supported with respect to equipment, facilities, and
budget. Supported by both core NIST funding and other agency funding, the division
maintains an appropriate balance between the goals of making progress on longer-term
problems not amenable to quick solutions and producing results in current areas of interests
that enhance the profile of NIST. The morale of the SMSD staff is positive. The researchers
are dedicated to the goals mentioned above. This division is an important national resource.
RESPONSE TO RECOMMENDATIONS FROM THE PREVIOUS REPORT
In the panel’s 2007 report,1 a few minor suggestions were given for further improving
the existing high-quality projects of the SMSD. These included better theoretical support for
projects involved in the detection of explosive materials, better definition and evaluation of
the health and safety risks of nanoparticles, improved theoretical understanding of cluster
secondary ion mass spectrometry (SIMS) of organic layers, more extensive collaborations in
the clean-room facility with experts on the synthesis and theory regarding the fabrication of
molecular electronics, and maintenance of the highly valuable data concerning surface
electron microscopy.
The majority of the suggestions have been accepted and implemented by the division.
For example, a detailed study that involves the preparation and quantitative analysis of
standard explosive samples was done. The fundamental properties of explosive molecules
have also become better understood since the 2007 review. The transport of nanoparticles in
biocells has been delineated. Sputter SIMS analysis of biomaterials was carried out. A
semitheoretical study of the organic thin-film transistors fabricated by a device group in
another NIST division has been completed. The highly popular x-ray-analysis database that
was based on the Apple computer system has been updated to a personal computer system.
Additional work on theory, modeling, and simulation should be done, perhaps in collaboration
with experts in other divisions of NIST.
1
National Research Council, An Assessment of the National Institute of Standards and Technology
Chemical Science and Technology Laboratory: Fiscal Year 2007. Washington, D.C.: The National Academies
Press, 2007.
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TECHNICAL MERIT
The two major objectives of the Surface and Microanalysis Science Division are the
development of metrology technology and fundamental scientific research. For the former,
five representative topics were demonstrated to the panel. These are as follows: the
identification of uranium (U) isotopes, the detection of trace amounts of explosive materials,
chemical mapping by desorption mass spectrometry, the tracking and removal of
nanoparticles in aquatic environments, and the correlation of cracks in concrete with chemical
mapping by high-resolution transmission electron microscopy (TEM). For the latter, three
representative topics were shown: chemical imaging of individual nanostructures,
mechanisms of charge transfer in molecular nanoelectronics, and super-resolution leading to
significantly improved optical microscopy. The division’s scientific program appears to be
larger than that for technology development simply because the scientific projects have more
subtopics. However, the technical studies are well targeted at solving problems in national and
international security, environmental protection and sustainability, and transportation
infrastructure. All of these are national priorities with high impact and high visibility.
The scientific studies are spread over a wide range of fields in chemistry, bioscience,
optics, electronics, materials, and nanotechnology. The accurate identification of trace
isotopes of U is unique and critical to DHS and International Atomic Energy Agency (IAEA)
missions. The development of trace-detection metrology for explosives is important to
national security. For this purpose, a detailed method for the preparation of standard samples
has been investigated. The need now is to establish expected sample lifetimes. The integration
of chemical analysis techniques would also be beneficial.
The work on high-throughput, site-specific chemical mapping by SIMS is of practical
value to airport security. The reliability of the process and the long-term effects on health may
need investigation.
The quantitative chemical imaging of individual nanostructures by TEM is interesting
and potentially important for applications to both safety and the environment. It may also
have benefit for potential applications to microelectronic devices—for example, in helping to
understand Si/high-k-dielectric interfaces. The focus on the development of robust methods of
analysis and energy-dispersive techniques for aberration-corrected TEM (in contrast to efforts
in electron-energy-loss spectroscopy in other national laboratories) is consistent with the
NIST mission of metrology development.
The project on studying engineered nanoparticles in aquatic environments is
potentially important for water purification. An effective agent, such as a chelator, may help
in separating carbon nanotubes from the aquatic environment.
The cadmium selenide (CdSe) quantum-dot project, measuring the trophic transfer of
nanoparticles in a simplified invertebrate food web, indicates that the biomagnification of
nanoparticles, or at least particular types of nanoparticles, may not represent a health hazard.
A further study on why the nanoparticles do not accumulate will enhance the visibility of this
project.
The fast TEM imaging on the formation of cracks in concrete is very good work with
practical value. A detailed analysis of the connection between the chemical distribution and
crack formation would be an excellent scientific study. More generally, by addressing the
analysis of large specimens and connecting micro and macro properties of complex materials,
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this work can have a broad impact on detailed characterization and its relationship to the
performance properties of a wide variety of complex materials.
The work on charge-transfer mechanisms and the probing of surface potentials in
nanoelectronics is interesting. The emphasis on developing reliable methods and databases for
molecular electronics is appropriate in view of the NIST mission.
When completed, the project involving super-resolution optical microscopy will have
particularly high impact. The principal investigator has already published several excellent
papers on this subject.
The overall technical quality of the division is very good, with many projects being
among the best. However, the impact of SMSD’s work could be enhanced significantly
without the need for major additional resources by adding theoretical support to some of the
experimental projects. This could be accomplished, for example, by initiating collaborations
with outside organizations. It is encouraging that many of the research projects already
involve other divisions in NIST; external government agencies such as the U.S. Air Force,
Department of Homeland Security, National Institutes of Health, National Cancer Institute,
Food and Drug Administration, Savannah River National Laboratory, and various Army
laboratories; industry, including General Electric and SEMATECH; and universities such as
the University of Maryland, Pennsylvania State University, and the University of Kentucky.
Given the present imbalance between the number of technical staff and the relatively large
amount of state-of-the-art equipment, the impact of the division could be made even more
impressive by establishing more collaboration with outside organizations such as universities
or national laboratories. It can also be anticipated that such collaborations would bring in
fresh ideas, and the existing excellent infrastructure would be used to explore new territory.
A division-wide strategy needs to be developed to enhance the visibility of the SMSD
and its impact in the government and scientific communities, because this division includes a
wide range of activities. Some projects can benefit from an improved definition of strategy,
such as the long-term direction of scientific study and technology development. The division
should also promote worthy investigators for external recognition in the form of prizes and
awards.
The scientific staff of the division is highly productive. For example, in fiscal year
(FY) 2008, division researchers produced 55 manuscripts for publication, made 118
presentations that included 53 invited talks, filed for 1 patent, received 3 awards including 1
fellowship, and participated on 110 committees, including serving as committee leaders.
Every member of the scientific staff is involved in the publication and presentation process,
with a few members compiling outstanding records. On average, each member of the
scientific staff published 1.7 papers and delivered 3.5 talks. This is an excellent record, which
shows that the division is meeting its mandate to make a difference in scientific and technical
areas.
INFRASTRUCTURE AND SUPPORT
Compared with most university and industrial research laboratories, the Surface and
Microanalysis Science Division has some outstanding experimental equipment. Most of it
can be considered top of the line. Laboratory space, utilities, and safety features are all
significantly better than what is found in many other laboratories. Although the equipment
may not be used to full capacity, as noted above, the scientific and supporting staff engaged in
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the research and service programs are outstanding. The use of additional graduate and
undergraduate students in the summer is also a positive strategy whose continuation is
encouraged. The $12.5 million budget of the division, averaging out to $367,000 per staff
member, not including other agency equipment funds, is as good as, or even better than, that
found in first-class high-technology companies. The major portion of the budget is for
scientific and technical research activities for NIST and other agencies of the U.S.
government, showing the scientific importance of the division’s work. About one-third of the
portfolio is dedicated to programs related to public safety, security, and standards, showing
the commitment of the division to one of the most important goals of NIST. Division staff
identified no complaints about the lack of personnel, budget, equipment, or space to carry out
projects. Therefore, this is a well-supported division with no obvious deficiencies in
infrastructure.
OBJECTIVES AND IMPACT
The general goal of the SMSD is to serve the nation in areas of chemical metrology,
research, standards, and data. The specific goals are to characterize the spatial and temporal
distribution of chemical species and to improve the accuracy, precision, sensitivity,
selectivity, and applicability of surface, interface, microanalysis, and advanced isotope-
measurement techniques. The division carries various activities in order to accomplish these
goals satisfactorily. Its work in chemistry metrology includes the detection of trace narcotics,
the development of drug-delivery systems, the determination of molecular-orbital structure,
and the electronic structure of organic electronics. Its research activities include the
adsorption of self-assembled monolayers of nonspecific proteins, spectrometry using
supercontinuum sources, the imaging of surface potentials of organic thin-film transistors, the
transfer of quantum dots in an invertebrate food web, and super-resolution optical
microscopy. Its work in standards development includes the preparation of polymer
microspheres containing explosives, precision measurements of isotope ratios, and chemical
mapping. Its data activities include reinvention of the Desk Top Spectrum Analyzer and the
x-ray spectral imaging of cracks in bridges.
This work has demonstrated that the objectives of the division are being fulfilled
successfully owing to the effort of its dedicated staff and the availability of the state-of-the-art
equipment. The results can be anticipated to have major impacts on national security, the
overall mission of NIST, and the scientific community.
CONCLUSIONS
The Surface and Microanalysis Science Division has successfully accomplished its
own targets as well as those of NIST in serving the nation in areas of chemical metrology,
research, standards, and data. Many of the scientific studies of the SMSD have achieved
excellent results that have, for example, enhanced the capability to characterize surfaces and
interfaces with increased accuracy and precision. The division has a competent technical staff
with state-of-the-art equipment, advanced facilities, and sufficient budget. To further enhance
the capability of the division to achieve its objectives and have more impact on the scientific
community, those involved may wish to consider ways of expanding the division’s
collaborations with universities and national laboratories so as to make better use of its
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facilities and bring in fresh ideas as well as initiate explorations in new areas. Another path to
improving the division’s effectiveness is to bring in more theoretical experts, both within
NIST and externally, for more in-depth interpretation of some of SMSD’s excellent
experimental data. A further area of possible improvement for some projects is a better
definition of strategy, such as the long-term direction of scientific study and technology
development. Since this division includes a wide range of activities, the development of a
division-wide strategy could lead to greatly enhanced visibility and impact in the government
and scientific communities.
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