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SURFACE MAPPING MICROANALYSIS

Description:

 

6.     surface mapping MICROANALYSiS

Maximum Phase I Award Amount: $200,000

Maximum Phase II Award Amount: $1,100,000

Accepting SBIR Phase I Applications: YES

Accepting STTR Phase I Applications: NO

 

Nuclear forensics analysis often involves combining information from several microanalytical imaging technologies (e.g., optical microscopy, scanning electron microscopy [SEM], secondary ion mass spectrometry [SIMS], and other spectroscopic methods) in a serial fashion to provide a complete characterization of material samples. A significant challenge for analytical imaging technologies is the characterization of a single region of interest by complementary methods, which requires precise sample positioning, identification of features that warrant analysis by different analytical techniques, relocation of regions or features with high accuracy (typically within a few micrometers) on different analytical platforms, correlation of analytical signals from disparate technologies (e.g., reflected light, secondary electrons or ions, x-ray fluorescence, etc.), and visualization (e.g., 2-D or 3-D surface mapping). Therefore, of interest to DNN R&D are innovative solutions to (i) rapidly scan surfaces using various microscopies, (ii) efficiently correlate microanalytical images that provide complementary information, (iii) combine images so that they correctly align, and (iv) enable 2-D and 3-D surface mapping that combine disparate analytical data. Regions of interest can require cross-platform spatial resolution of one micrometer or less. For example, features of interest can be identified by rapid scanning using one or more imaging techniques (e.g. optical, SEM, SIMS, etc.); regions are relocated on a separation analytical platform for further analysis at short length scales; disparate information streams (e.g., chemical, elemental, isotopic, morphologic) are correlated to align or overlay features at high spatial resolution; and finally, optical images are then utilized to develop a 2-D or 3-D surface map combining all analytical information. Research is needed to achieve rapid scanning and spatial alignment of surface maps made by each microscopy to the same x-y-z position. Materials of interest may be affixed to sample holding substrates made of various materials (e.g., glass, carbon, plastic, silicon, gold, aluminum, or steel). Thermal stability, electrical conductivity, material compatibility, and stability all must be maintained, such that regions of interest can be archived and reanalyzed as needed. Approaches should enable the ability to identify and target key features, to include but not limited to: trace surface contamination, particle grain inclusions, surface treatments, signs of aging or corrosion, and radiolytic damage.

 

Grant applications are sought in the following subtopics:

 

a.      Rapid Scanning and Feature Discrimination

Research in rapid scanning of SNM surfaces is needed to image and identify down to sub-micron resolution unusual features (e.g., defects, areas of anomalous composition, or material inclusions) on samples of special nuclear material (SNM) or surrogates (e.g., cerium oxide or depleted uranium samples). Technology developed in this subtopic is of value to either (i) enable scans of surfaces (ideally 1 sq. cm area) using various microscopies (electron, optical, other) at high resolution (ideally micron or sub-micron resolution) rapidly (ideally hours or days rather than years to complete a high-resolution scan of such a large surface area), or (ii) enable scans of surfaces (ideally 1 sq. cm area) using various microscopies (electron, optical, other) at relatively low resolution rapidly, then apply algorithms to select subsample spots for micron-scale imaging. Software algorithms developed in this subtopic could be used to locate micron-sized particles of interest (e.g., dust or pollen grains) or regions of abnormality for further scrutiny and analysis. This subtopic welcomes rapid approaches that facilitate the determination of whether a single mapped square cm area is truly representative of the entire sample surface, as well as probe whether a subsample image exhibits correlated pattern templates representing the full area under investigation.

 

Questions – Contact: Timothy Ashenfelter, Timothy.Ashenfelter@nnsa.doe.gov

 

b.      2-D and 3-D Surface Mapping Across Multiple Microscopy Platforms

Research is needed in machine vision approaches that correlate features in the spatial fields-of-view between optical microscopy platforms and analytical images obtained by other means such as SEM, SEM-Energy Dispersive Spectrometry (EDS), and SIMS. Software algorithms and/or instrumentation developed in this subtopic is of value to enable (i) scans of surfaces using various microscopies (e.g., electron or optical), (ii) image correlation to align and overlay images from combinations of imaging platforms, (iii) accurate indexing of features of interest on microscopy platforms to resolutions of 1 micrometer or better, and/or (iv) 3-D mapping of surface topography to assess surface uniformity as a function of position. Sample substrates typically require conductive materials such as metal-coated glass, silicon, or carbon and require registration at or better than the one-micrometer scale. Techniques are desired to assess surface uniformity, curvature, or address morphology as a function of position, for optically rough surfaces of the order of one square centimeter.

 

Questions – Contact: Timothy Ashenfelter, Timothy.Ashenfelter@nnsa.doe.gov

 

c.       Spatial Alignment and Target Extraction

Research is needed to develop an optical inspection and robust sample manipulation stage for the removal of particulates of typical diameter 1-300 micrometers from an oxide or metal surface. The functionality of interest is that of a stage of an optical microscope, with manipulation capable of at least four degrees of freedom (DOF) – e.g., x, y, z sample movement and z movement of a particle removal mechanism – with sub-micrometer reproducible positioning. In our application, sample removal mechanisms must utilize methods that do not alter the chemical composition of the particulates or transfer contamination so that ultra-trace destructive analyses can be performed to characterize the chemical and isotopic composition of collected particles. Materials of interest are solid samples comprised of both refractory materials (e.g., SiO2, Al2O3, and similar oxides) and light elements (i.e., low-Z organic macromolecules). Also of interest are techniques that provide a 3-D visualization of the extracted component.

 

Questions – Contact: Timothy Ashenfelter, Timothy.Ashenfelter@nnsa.doe.gov

 

 

d.      Other

In addition to the specific subtopics listed above, grant applications are sought in other areas that fall within the scope of the topic description above.

 

Questions – Contact: Timothy Ashenfelter, Timothy.Ashenfelter@nnsa.doe.gov

 

References: Subtopic a:

1.      Nelson, M. P., Zugates, C. T., Treado, P. J., Casuccio, G. S., Exline, D.L., & Schlaegle, S. F. “Combining Raman Chemical Imaging and Scanning Electron Microscopy to Characterize Ambient Fine Particulate Matter.” Aerosol Science & Technology, Vol. 34, Issue 1, pp. 108-117, 2001, DOI: 0.1080/02786820120709, 2001, https://www.researchgate.net/publication/239792090_Combining_Raman_Chemical_Imaging_and_Scanning_Electron_Microscopy_to_Characterize_Ambient_Fine_Particulate_Matter

 

2.      Schaaff, T.G., McMahon, J.M., and Todd, P.J. “Semiautomated analytical image correlation.” Analytical Chemistry, Volume 74, Pages 4361-4369, https://www.researchgate.net/publication/11155045_Semiautomated_Analytical_Image_Correlation

 

3.      Masyuko, R.; Lanni, E.J.; Sweedler, J.V.; Bohn, P.W. “Correlated imaging – A grand challenge in chemical analysis.” Analyst, Volume 138, pages 1924-1939, 2003, https://www.ncbi.nlm.nih.gov/pmc/articles/PMC3718397/

 

4.      Park, Y. J., Song, K., Pyo, H. Y., Lee, M.H., Jee, K.Y., Kim, W. H. “Investigation on the fission track analysis of uranium-doped particles for the screening of safeguards environmental samples.” Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Volume 557, Issue 2, 15 February 2006, Pages 657-663, https://www.sciencedirect.com/science/article/pii/S0168900205023144

 

References: Subtopic b:

1.      Gong, Z., et al. “Fluorescence and SEM correlative microscopy for nanomanipulation of subcellular structures.” Light: Science & Applications, 2014, 3, e224, doi: 10.1038/lsa.2014.105, https://www.nature.com/articles/lsa2014105

 

2.      Zimmermann, S.; Tiemerding, T.; Fatikow, S. “Automated robotic manipulation of individual colloidal particles using vision-based control.” IEEE-ASME Trans. Mechatronics Volume 20, Issue 5, pp 2031-2038, 2014, DOI: 10.1109/TMECH.2014.2361271, https://www.researchgate.net/publication/273336412_Automated_Robotic_Manipulation_of_Individual_Colloidal_Particles_Using_Vision-Based_Control

 

3.      Pinskier, J.; Shirinzadeh, B.; Clark, L.; Qui, Y. “Development of a 4-DOF haptic micromanipulator utilizing a hybrid parallel serial flexure mechanism.” Mechatronics, Volume 50, pp 55-68 (2018) DOI: 10.1016/j.mechatronics.2018.01.007, https://www.sciencedirect.com/science/article/abs/pii/S0957415818300072

 

4.      Curtis, M. Farago, F. “Handbook of Dimensional Measurement, Fifth Edition.” Industrial Press Inc., 656 pages, 2013, https://www.amazon.com/Handbook-Dimensional-Measurement-Mark-Curtis/dp/0831134658

 

 

References: Subtopic c:

1.      Herranen, J., Markkanen, J., Videen, G., Muinonen, K. “Non-spherical particles in optical tweezers: A numerical solution.” PLoS ONE 14(12): e0225773, 2019, https://doi.org/10.1371/journal.pone.0225773

 

2.      Polemeno et al, Optical tweezers and their applications, Journal of Quantitative Spectroscopy and Radiative Transfer (2018). Vol 218, pp 131-150 https://www.sciencedirect.com/science/article/abs/pii/S002240731830445X

 

3.      Brandon C.W., Erler, R.G., and Teslich, N.E. “Three-dimensional microstructural characterization of bulk plutonium and uranium metals using focused ion beam technique.” United States: N. p., 2016. Web. doi:10.1016/j.jnucmat.2016.01.0, https://www.sciencedirect.com/science/article/abs/pii/S0022311516300290

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